Influence of Oleic Acid Modified Ultrafine Cement on Performance of Grouting Materials

doi:10.16552/j.cnki.issn1001-1625.2026.0054

Abstract

Abstract:

In the repair of concrete micro-cracks， ultrafine cement （UPC） faces the problems of poor slurry fluidity， high porosity and susceptibility to dissolution under low water-cement ratio. In this study， the surface modification of UPC with oleic acid was proposed to simultaneously improve its injectability and hydrophobicity. Oleic acid modified UPC with oleic acid content of 0%~0.3% （mass fraction） was prepared by ball milling method. The rheological properties， compressive strength， heat of hydration， hydrophobic properties and interfacial bond strength of the modified UPC paste were systematically evaluated， and the modification mechanism was revealed by FTIR， SEM， TG， LF-NMR. The results show that appropriate amount of oleic acid （0.1%） modification can reduce the viscosity of grouting material and improve the rheological properties. At the same time， at this dosage， the inhibition effect on cement hydration is small， the strength of the slurry is not much affected， and the autogenous shrinkage of the slurry is significantly reduced. Oleic acid is involved in the surface modification of cement particles， and the contact angle of hardened slurry increases from 48.6° to 126.4°. However， an excessive amount of oleic acid （>0.2%） severely inhibits the hydration reaction， reduces the 28 d compressive strength from 54.95 MPa to 23.08 MPa， and increases the autogenous shrinkage and porosity. In this paper， the study investigates the action mechanism and dosage threshold of oleic acid in UPC， which provides support for the development of high-performance microfracture anti-seepage repair materials.

Key words: ultrafine cement, oleic acid, hydrophobicity, hydration process, pore structure

CLC Number:

TU528

CAO Yujie, LIU Lv, HUANG Dong, HUANG Chaoqun, LIU Yunpeng. Influence of Oleic Acid Modified Ultrafine Cement on Performance of Grouting Materials[J]. BULLETIN OF THE CHINESE CERAMIC SOCIETY, 2026, 45(7): 2226-2236.

Figures/Tables 17

Table 1 Chemical composition of ultrafine cement

Chemical composition	SiO₂	CaO	Al₂O₃	Fe₂O₃	MgO	SO₃	K₂O	Na₂O	TiO₂	LOl
Mass fraction/%	22.93	60.65	4.23	3.05	4.01	2.56	0.46	0.23	0.47	1.41

Table 2 Physical properties of ultrafine cement

Indicator	Flexural strength/MPa			Compressive strength/MPa			Setting time/min
Indicator	3 d	7 d	28 d	3 d	7 d	28 d	Initial	Final
Value	7.10	8.35	9.10	27.40	44.80	59.70	125	195

Table 3 Basic mix ratio of grouting material

Sample	Mass/g			W/C
Sample	UPC	Water	OA	W/C
S	200	100	0	0.5
A	200	100	0.2	0.5
B	200	100	0.4	0.5
C	200	100	0.6	0.5

Fig.1 Influence of oleic acid addition on particle size of ultrafine cement

Fig.2 Interface bonding strength test

Fig.3 Effect of different oleic acid content on rheological properties of ultrafine cement paste

Table 4 Fitting results of rheological parameters based on Herschel-Bulkley model

Sample	W/C	Herschel-Bulkley model	τ₀/Pa	n	R²/%
S	0.5	y=23.52+3.82x^0.57	23.52	0.57	99.96
A	0.5	y=23.93+0.56x^0.47	23.93	0.47	99.68
B	0.5	y=24.91+2.52x^0.62	24.91	0.62	99.94
C	0.5	y=36.57+0.69x^0.74	36.57	0.74	99.68

Fig.4 Water contact angles of UPC with different oleic acid content

Fig.5 FTIR spectra of UPC with different oleic acid content

Fig.6 Influence of oleic acid content on compressive strength of UPC grouting materials

Fig.7 Influence of different oleic acid content on hydration process of UPC

Fig.8 TG-DTG and Ca（OH）2 weight loss of different oleic acid modified ultrafine cement

Fig.9 SEM images of UPC with different oleic acid content

Fig.10 Interfacial bonding strength of specimens

Fig.11 Influence of oleic acid content on shrinkage of ultrafine cement pastes with different oleic acid content

Fig.12 Distribution of T2 relaxation time of UPC in different groups within 24 h

Fig.13 Evolution of T2 relaxation time distribution of each group of UPC under different curing ages

References 25

[1]	鲁晨，范银琴. 地下连接通道渗漏水治理施工技术研究［J］. 建筑施工， 2025， 47（12）： 1842-1846.
	LU C， FAN Y Q. Study on construction techniques for water leakage treatment in underground connecting channels［J］. Building Construction， 2025， 47（12）： 1842-1846 （in Chinese）.
[2]	刘江峰，王锐，孟庆彬，等. 超细水泥生产工艺、性能及工程应用研究进展［J］. 硅酸盐通报， 2023， 42（5）： 1519-1528.
	LIU J F， WANG R， MENG Q B， et al. Research progress on production technology， properties and engineering application of superfine cement［J］. Bulletin of the Chinese Ceramic Society， 2023， 42（5）： 1519-1528 （in Chinese）.
[3]	HAN J Y， WANG J， YANG W K， et al. Experimental study on the properties of a polymer-modified superfine cementitious composite material for waterproofing and plugging［J］. Case Studies in Construction Materials， 2023， 19： e02552.
[4]	ZHAO J J， TIAN S X， CHEN C， et al. Research on the performance and application of nano-MgO modified ultrafine cement-based sealing materials［J］. Case Studies in Construction Materials， 2025， 22： e04694.
[5]	赵卫全，任增增，张金接，等. 超细水泥-硅灰二元低pH注浆材料特性研究［J］. 硅酸盐通报， 2023， 42（4）： 1156-1165.
	CHAO Q W， REN Z Z， ZHANG J J， et al. Characteristics of binary low-pH grouting material containing superfine cement and silica fume［J］. Bulletin of the Chinese Ceramic Society， 2023， 42（4）： 1156-1165 （in Chinese）.
[6]	张培森，李腾辉，赵成业，等. 高强度低粘度注浆材料配比试验研究［J］. 煤炭工程， 2021， 53（3）： 145-150. DOI
	ZHANG P S， LI T H， ZHAO C Y， et al. Proportioning test of high strength and low viscosity grouting materials［J］. Coal Engineering， 2021， 53（3）： 145-150 （in Chinese）.
[7]	王伟伟，韩健勇，朱士豪. 复合超细水泥基防水堵漏材料性能及聚合物改性影响研究［J］. 新型建筑材料， 2025， 52（6）： 97-100.
	WANG W W， HAN J Y， ZHU S H. Study on properties of composite superfine cement-based waterproof plugging material and influence of polymer modification［J］. New Building Materials， 2025， 52（6）： 97-100 （in Chinese）.
[8]	LANZÓN M， GARCÍA-RUIZ P A. Effectiveness and durability evaluation of rendering mortars made with metallic soaps and powdered silicone［J］. Construction and Building Materials， 2008， 22（12）： 2308-2315. DOI URL
[9]	冯明月，杨旭，谢恬静，等. 表面修饰材料制备疏水油井水泥的性能评价［J］. 油田化学， 2022， 39（3）： 413-417.
	FENG M Y， YANG X， XIE T J， et al. Performance evaluation of hydrophobic oil well cement prepared by surface modification materials［J］. Oilfield Chemistry， 2022， 39（3）： 413-417 （in Chinese）.
[10]	冯传法. 水泥基材料疏水及表面超疏水改性研究［D］. 武汉：武汉理工大学， 2018.
	FENG C F. Study on hydrophobic and surface superhydrophobic modification of cement-based materials［D］. Wuhan： Wuhan University of Technology， 2018 （in Chinese）.
[11]	杜亮波，周伟林，刘加平，等. 水泥助磨剂的研究进展［J］. 材料导报， 2009， 23（21）： 80-84.
	DU L B， ZHOU W L， LIU J P， et al. Research progress of cement grinding aids［J］. Materials Review， 2009， 23（21）： 80-84 （in Chinese）.
[12]	ZHANG C Y， WANG M， LIU R T， et al. Rheological properties of cement-based slurry and evaluation of rheological model： influence of particle size and shape［J］. Construction and Building Materials， 2023， 406： 133498. DOI URL
[13]	SHA F， KONG H， ZHANG L Y， et al. Rheological properties of CEMI type microfine cement slurry with different fineness ［J］. Construction and Building Materials， 2023， 404： 133253. DOI URL
[14]	LIU P， FENG C F， WANG F Z， et al. Hydrophobic and water-resisting behavior of Portland cement incorporated by oleic acid modified fly ash［J］. Materials and Structures， 2018， 51（2）： 38. DOI
[15]	LU B， SHI C J， ZHANG J K， et al. Effects of carbonated hardened cement paste powder on hydration and microstructure of Portland cement［J］. Construction and Building Materials， 2018， 186： 699-708. DOI URL
[16]	HE X， DE LOS REYES F L III， LEMING M L， et al. Mechanisms of fat， oil and grease （FOG） deposit formation in sewer lines［J］. Water Research， 2013， 47（13）： 4451-4459. DOI URL
[17]	MEKONNEN K D. Fourier transform infrared spectroscopy as a tool for identifying the unique characteristic bands of lipid in oilseed components： confirmed via Ethiopian indigenous desert date fruit［J］. Heliyon， 2023， 9（4）： e14699.
[18]	TUGRUL ALBAYRAK A， YASAR M， GURKAYNAK M， et al. Investigation of the effects of fatty acids on the compressive strength of the concrete and the grindability of the cement［J］. Cement and Concrete Research， 2005， 35（2）： 400-404. DOI URL
[19]	周柏坊，孟祥瑞，王艳芬，等. 不同水灰比下矿用超细水泥注浆材料性能试验研究［J］. 采矿与岩层控制工程学报， 2025， 7（4）： 124-139.
	ZHOU B F， MENG X R， WANG Y F， et al. Performance of mine cement grouting materials with ultra-fine cement at different water-cement ratios［J］. Journal of Mining and Strata Control Engineering， 2025， 7（4）： 124-139 （in Chinese）.
[20]	韦华，李庆安，陈连军，等. 复合净浆对再生混凝土骨料性能影响及机理分析［J］. 水利水运工程学报， 2026（1）： 146-156.
	WEI H， LI Q A， CHEN L J， et al. Effect of composite cement paste on the properties of recycled concrete aggregate and its underlying mechanism［J］. Hydro-Science and Engineering， 2026（1）： 146-156 （in Chinese）.
[21]	刘伟，王乐威，易鹏，等. 低场核磁共振技术原理及其在水泥基材料中的研究进展［J］. 材料导报， 2025， 40（6）： 1-20.
	LIU W， WANG L W， YI P， et al. Principles of low-field nuclear magnetic resonance technology and emerging applications in cement-based materials ［J］. Materials Reports， 2025， 40（6）： 1-20 （in Chinese）.
[22]	王丹，薛善彬，白如飞，等. 基于低场核磁共振的硫铝酸盐水泥砂浆孔结构演变研究［J］. 硅酸盐通报， 2025， 44（3）： 852-861.
	WANG D， XUE S B， BAI R F， et al. Pore structure evolution of sulfoaluminate cement mortar based on low field nuclear magnetic resonance［J］. Bulletin of the Chinese Ceramic Society， 2025， 44（3）： 852-861 （in Chinese）.
[23]	乔晶，张笑与，张昀，等. 应用低场磁共振弛豫技术定量表征水泥基材料的研究进展［J］. 硅酸盐学报， 2025， 53（5）： 1339-1353.
	QIAO J， ZHANG X Y， ZHANG Y， et al. Application of low-field nuclear magnetic resonance relaxometry to characterize cement-based materials： a critical review［J］. Journal of the Chinese Ceramic Society， 2025， 53（5）： 1339-1353 （in Chinese）.
[24]	QIAO J， ZHOU C S， FENG J J， et al. ¹H LF-NMR study on water migration behavior of fresh cement paste with limestone powder［J］. Cement and Concrete Research， 2025， 191： 107802. DOI URL
[25]	LUO Q， HUANG J L. Mechanisms and critical technologies of transport inhibitor agent （TIA） throughout C-S-H nano-channels［J］. Materials， 2022， 15（2）： 515. DOI URL