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( 12 ) United States Patent US010150904B1 (12 ) United States Patent ( 10 ) Patent No. : US 10 , 150, 904 B1 Rahman et al. ( 45 ) Date of Patent : Dec . 11 , 2018 (54 ) NANO ZEOLITE CEMENT ADDITIVE AND ( 56 ) References Cited METHODS OF USE U . S . PATENT DOCUMENTS (71 ) Applicant : King Fahd University of Petroleum 6 , 989 ,057 B2 1 / 2006 Getzlaf et al. and Minerals , Dhahran (SA ) 8 , 940 ,670 B2 1 / 2015 Patil et al . 2004 / 0112600 A1 * 6 /2004 Luke . .. C04B 14 /047 ( 72 ) Inventors : Muhammad Kalimur Rahman , 166 /295 Dhahran (SA ) ; Mirza Talha Baig , 2007/ 0029088 A1* 2 / 2007 Di Lullo Arias .. .. C04B 14 / 047 Dhahran (SA ) ; Abdulaziz Al- Majed , 166 /292 2007 /0056732 A1 3 /2007 Roddy et al. Dhahran (SA ) 2014 /0332217 AL 11 /2014 Rahman et al . ( 73 ) Assignee : King Fahd University of Petroleum 2017/ 0240469 AL 8 / 2017 Rahman et al. and Minerals , Dhahran (SA ) OTHER PUBLICATIONS ( * ) Notice : Subject to any disclaimer, the term of this patent is extended or adjusted under 35 Mirza Talha Baig , et al. , “ Application of Nanotechnology in Oil U . S . C . 154 ( b ) by 0 days . Well Cementing ” , Society of Petroleum Engineers , SPE Kuwait Oil & Gas Show and Conference , Oct . 1 - 18 , Kuwait City , Kuwait , 2017 , ( 21 ) Appl. No .: 15 / 941, 350 pp . 1 - 3 . Hossein Mola - Abasi, et al ., “ Effect of Natural Zeolite and Cement Additive on the Strength of Sand ” , Geotechnical and Geological ( 22 ) Filed : Mar. 30 , 2018 Engineering, vol . 34 , Issue 5 , Oct . 2016 , pp . 1539 -1551 . (51 ) Int . CI. (Continued ) CO9K 8 / 46 ( 2006 .01 ) CO9K 8 / 467 ( 2006 .01 ) Primary Examiner — Catherine Loikith C04B 28 /02 ( 2006 .01 ) Assistant Examiner — Ashish K Varma C04B 28 /04 ( 2006 .01 ) ( 74 ) Attorney, Agent, or Firm — Oblon , McClelland , C04B 22 /06 ( 2006 . 01 ) Maier & Neustadt, L . L . P . C04B 14 / 04 ( 2006 . 01 ) E21B 33 / 14 ( 2006 . 01) (57 ) ABSTRACT ( 52 ) U . S . CI. The present invention discusses methods for making a CPC .. .. C09K 8 /467 ( 2013 .01 ) ; C04B 14 /043 cement composition comprising a nanoparticle zeolite . The (2013 .01 ) ; C04B 14 /047 ( 2013 .01 ) ; C04B addition of the nanoparticle zeolite may provide enhanced 22 / 064 ( 2013 .01 ) ; C04B 28 / 02 ( 2013 .01 ) ; compressive and tensile strengths, improved rheology , and a C04B 28 /04 ( 2013. 01) ; E21B 33/ 14 ( 2013 .01 ) ; change to the cement microstructure . These effects may COOK 2208/ 10 ( 2013 .01 ) improve the cement ' s use as a cement sheath in drilling ( 58 ) Field of Classification Search operations and under high pressure and high temperature CPC .. .. .. .. .. CO9K 8 / 467 ; E21B 33 / 14 (HPHT ) conditions . USPC .. .. .. 166 / 293 See application file for complete search history . 20 Claims, 14 Drawing Sheets QUIN US 10 ,150 ,904 B1 Page 2 ( 56 ) References Cited OTHER PUBLICATIONS Hossein Mola - Abasi , et al. , “ Influence of zeolite and cement addi tions on mechanical behavior of sandy soil ” , Journal of Rock Mechanics and Geotechnical Engineering , vol. 8 , Jun . 28 , 2016 , pp . 746 - 752 . Partha Sarathi Deb , et al. , " Effects of nano - silica on the strength development of geopolymer cured at room temperature ” , Construc tion and Building Materials , vol. 101 , Part 1 , Dec . 30 , 2015 , pp . 675 -683 . Alireza S . Khorasani , et al . , “ The Effects of Nanoparticles of Silica an Alumina on Flow Ability and Compressive Strength of Cementi tious Composites” , Key Engineering Materials ( /KEM ) , vol. 631 , Nov . 2014 , pp . 119 - 127 . Mirza Talha Baig , et al. , “ Evaluation of Nano Zeolite as an Additive for Oil -Well Cementing” , King Fahd University of Petroleum & Minerals , May 2017 , pp . 1 - 165 . * cited by examiner U . S . Patent Dec . 11 , 2018 Sheet 1 of 14 US 10 , 150 , 904 B1 wwwww DNEVNO 23 FIG . 1 U . S . Patent Dec . 11, 2018 Sheet 2 of 14 US 10 , 150, 904 B1 . ' ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . -. ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . ' . FIG . 2 U . S . Patent Dec . 11, 2018 Sheet 3 of 14 US 10 , 150, 904 B1 . 2300 is FIG . 3 U . S . Patent Dec . 11, 2018 Sheet 4 of 14 US 10 , 150, 904 B1 . FIG . 4 U . S . Patent Dec . 11, 2018 Sheet 5 of 14 US 10 , 150, 904 B1 . ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' . * * FIG . 5 U . S . Patent Dec . 11, 2018 Sheet 6 of 14 US 10 , 150, 904 B1 . WA 1 * WO ** * ** * WwW WWWXXNHIILITETI XOXO 94 O XXXXX * We 08 * DW * ** ** *** * * * ** * * * * ** * * ** 9824 ONLY 200 YEROR WS . KY. SEKSS3 it FIG . 6A XXX FIG . 6B U . S . Patent Dec . 11, 2018 Sheet 7 of 14 US 10 , 150, 904 B1 Www XXXX * * * XX 83 BA ** * *** * WWW w Atttttt** iiiitttt *** * * * * * * * * +1+ . 12 XWWWWWW w w FIG . 6C U . S . Patent Dec . 11, 2018 Sheet 8 of 14 US 10 , 150, 904 B1 Www W :. XXXXXX OX W LUX wwwWis XXXXX . FIG . 7A U . S . Patent Dec . 11, 2018 Sheet 9 of 14 US 10 , 150, 904 B1 Vw FIG . 7B U . S . Patent Dec . 11, 2018 Sheet 10 of 14 US 10 , 150 , 904 B1 IT XXXXXXXXXXXXXXXXXXXXX *222 AXA W0000 BRE WEBSCARVEST WWWWWW 392 XXXXXX FIG . 7C O DO SSSSSSSSSSS WWW COS wwwxxx WSXX XX FIG . 7D atent Dec . 11 , 2018 Sheet 11 of 14 US 10 , 150 , 904 B1 523nm SED 20KV FIG . 7E U . S . Patent Dec . 11, 2018 Sheet 12 of 14 US 10 , 150 , 904 B1 * * * XX ** * FIG . 7F U . S . Patent Dec . 11, 2018 Sheet 13 of 14 US 10 , 150 , 904 B1 XXX 10 WWW . *** * * * * ** ** ** * * ** * Www * * * XXX XXXXXXXXXXXXWww Speci, am 36 WWW*** * * ** * * * *F1 FIG . 8A U . S . Patent Dec . 11, 2018 Sheet 14 of 14 US 10 , 150 , 904 B1 wwww CD wwwwwwww Woo oooooooo WWWWW ORE WWWWWWWWWWOXXXXXXXXXXXWWWWWXXXXXXXXX FIG . 8B O W XXXXXXXXXXXXXXXXX XXX MWASA ANAK XXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXX WWWXX FIG , 8C US 10 , 150 ,904 B1 NANO ZEOLITE CEMENT ADDITIVE AND fluid in liquid or gaseous form through or at the boundaries METHODS OF USE of the cement sheath . The zonal isolation requires a robust cement slurry which provides a strong and durable cement STATEMENT REGARDING PRIOR casing and cement- formation bonding , precludes bulk DISCLOSURES BY THE INVENTORS 5 shrinkage by inhibiting the fluid loss, has zero free water settling of cement, and does not form a micro annulus due Aspects of this technology were disclosed in a thesis to stress imbalance at the interface resulting from thermal defense titled , “ Evaluation of Nano zeolite as an Additive for regimes, hydraulic pressure or mechanical stresses . The Oil - Well Cementing , ” presented by Baig . Mirza Talha on hardened cement slurry should also resist radial fracturing May 25 , 2017 at King Fahd University of Petroleum & 10 that may result from shrinkage stresses, thermal expansion Minerals (KFUPM ) , Dhahran , Saudi Arabia , and is herein or contraction of the steel casing and pressure fluctuation , incorporated by reference in its entirety . mechanical impact, or other conditions within the casing . The HPHT wells have a larger probability of migration of BACKGROUND OF THE INVENTION gas and corrosive fluid and leakage . Therefore , special attention must be paid to cementing processes, especially in Technical Field HPHTwells . Studies have shown that approximately 80 % of the wells in the Gulf of Mexico have gas transmitted to the The present invention relates to a method of making a surface through the cement casing. cured cement material comprising a nanoparticle- sized zeo In HPHT formations , the wells are exposed to high lite . 20 temperature variations that unsettle the formation as well as the casing , initiating expansion and contraction . In addition , Description of the Related Art HPHTwells are subjected to high loads in the lifetime of the well ; this may destroy the integrity of cement and may The “ background ” description provided herein is for the produce cracks due to compaction loads. Gas migration and purpose of generally presenting the context of the disclo - 25 strength retrogression are major challenges in HPHT well sure . Work of the presently named inventors , to the extent it cementing . is described in this background section , as well as aspects of Gas migration is one of the major failures of primary the description which may not otherwise qualify as prior art cementing jobs resulting in loss of production and requires at the time of filing , are neither expressly or impliedly costly remedial cementing jobs to fix the well. One of the admitted as prior art against the present invention . 30 major causes behind the Gulf of Mexico oil spill incident Oil and gas production and its exploration influence the was the poor cementing job ; in that incident the annulus world ' s economic structure . Conventional petroleum reser - cement barrier could not stop the flow of hydrocarbons . voirs are being exhausted because of the increase in eco - Some important cement properties such as , free water, fluid nomic activity in recent decades . To bridge the gap between loss , and static gel - strength transition time, were not evalu supply and demand of petroleum products , engineers are 35 ated prior to the cementing job . See Garg , T . , & Gokavarapu , now exploring reserves which were neglected in the past due S . ( 2012 ) . Lessons Learnt from Root Cause Analysis of Gulf to various complications associated with extraction . Tech - of Mexico Oil Spill 2010 , (December ), 10 - 12 , incorporated nological advancements in the field of petroleum engineer - herein by reference in its entirety . Most HPHT environments ing have now enabled researchers to cope with the problems are in gas production horizons , so it is a major concern in efficiently and improve the overall success of operations . To 40 HPHT wells as gas may migrate through the cement micro exploit the unconventional resources of petroleum , new cracks . See Shaughnessy , J . , & Helweg , J . ( 2002 ) . Optimiz techniques must be established simultaneously with an ing HTHP Cementing Operations . IADC /SPE Drilling Con improvement in existing techniques . ference , 26 - 28 February , Dallas , Tex . IADC /SPE - 74483 In oil and gas wells after drilling the wellbore is com MS.
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