Synthesis and properties of high temperature retarder HJ-1

doi:10.16085/j.issn.1000-6613.2024-1030

Abstract

Abstract:

AMPS-IA, AMPS-IA-MA and AMPS-IA-NNDMA were synthesized from 2-acrylamide-2-methylpropanesulfonic acid (AMPS), itaconic acid (IA), maleic acid (MA) or N,N-dimethylacrylamide (NNDMA) by free radical aqueous copolymerization method. The results showed that the thermal stability of AMPS-IA-MA was significantly higher than that of the other two and the initial decomposition temperature was as high as 343℃. It was found that the cement slurry with retarder had good temperature resistance and retarding effect. When combined with borax (PS), the thickening and rheological properties of cement slurry were further improved and the compressive strength of cement stone was basically unchanged. Under the conditions of 180℃ and 30MPa, the thickening time reaches 260min and the strength of cement stone after curing for 24h and 72h was 23.75MPa and 20.69MPa, respectively.

Key words: hot dry rock, retarder, copolymer, thermal stability

摘要：

以2-丙烯酰胺基-2-甲基丙磺酸（AMPS）、衣康酸（IA）、顺丁烯二酸（MA）或N,N-二甲基丙烯酰胺（NNDMA）为原料，采用自由基水溶液共聚法合成AMPS-IA、AMPS-IA-MA、AMPS-IA-NNDMA三种缓凝剂。结果表明，AMPS-IA-MA的热稳定性明显高于其他两种，起始分解温度高达343℃。水泥浆稠化实验研究发现加有缓凝剂的水泥浆表现出良好的抗温缓凝效果。当与硼砂复配使用时，进一步提升了水泥浆的稠化性能和流变性能，同时水泥石抗压强度保持不变。180℃、30MPa条件下，稠化时间达260min，养护24h和72h后水泥石强度分别为23.75MPa和20.69MPa。

关键词: 干热岩, 缓凝剂, 共聚物, 热稳定性

CLC Number:

TQ172

LI Zhifu, YANG Xiaodong, WANG Baocai, HU Changliu, PEI Jikai, YAN Longfang, WU Ruifang, ZHANG Changsheng, WANG Yongzhao. Synthesis and properties of high temperature retarder HJ-1[J]. Chemical Industry and Engineering Progress, 2025, 44(9): 5092-5100.

李志福, 杨晓东, 汪保财, 胡长流, 裴继凯, 阎龙芳, 武瑞芳, 张昌生, 王永钊. 耐高温缓凝剂HJ-1的合成及性能[J]. 化工进展, 2025, 44(9): 5092-5100.

Figures/Tables 13

References 21

[1]	WANG Yuqing, LIU Yingxin, DOU Jinyue, et al. Geothermal energy in China: Status, challenges, and policy recommendations[J]. Utilities Policy, 2020, 64: 101020.
[2]	HE Yujiang, BU Xianbiao. Performance of hybrid single well enhanced geothermal system and solar energy for buildings heating[J]. Energies, 2020, 13(10): 2473.
[3]	PYATINA Tatiana, SUGAMA Toshifumi. Cements with supplementary cementitious materials for high-temperature geothermal wells[J]. Geothermics, 2020, 86: 101840.
[4]	BERGEN Sophia L, ZEMBEREKCI Lyn, NAIR Sriramya Duddukuri. A review of conventional and alternative cementitious materials for geothermal wells[J]. Renewable and Sustainable Energy Reviews, 2022, 161: 112347.
[5]	TANG Xin, YANG Yan, HU Xuzeng. Retarder design for long open-hole well cementing through the interfacial adsorption[J]. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 2023, 677: 132278.
[6]	BIAN Jifa, YE Zhongbin, ZHENG Xuecheng, et al. High-temperature resistant copolymer oil well cement retarder: Synthesis, assessment of performance, and mechanism of retardation[J]. Journal of Applied Polymer Science, 2024, 141(18): e55316.
[7]	宋茂林, 耿国伟, 王云庆, 等. 一种高温低敏感油井水泥缓凝剂H37的室内研究[J]. 中国石油和化工标准与质量, 2020, 40(1): 94-95.
	SONG Maolin, GENG Guowei, WANG Yunqing, et al. Laboratory study on a high temperature and low sensitivity retarder H37 for oil well cement[J]. China Petroleum and Chemical Standard and Quality, 2020, 40(1): 94-95.
[8]	CONSTANTIN Tiemeyer, JOHANN Plank. Working mechanism of a high temperature (200℃) synthetic cement retarder and its interaction with an AMPS^®-based fluid loss polymer in oil well cement[J]. Journal of Applied Polymer Science, 2012, 124(6): 4772-4781.
[9]	李晓岚, 郑志军, 郭鹏. 高温油井水泥缓凝剂ZRT-1的合成及性能[J]. 钻井液与完井液, 2020, 37(1): 93-96.
	LI Xiaolan, ZHENG Zhijun, GUO Peng. Synthesis and performance evaluation of high temperature oil well cement retarder ZRT-1[J]. Drilling Fluid & Completion Fluid, 2020, 37(1): 93-96.
[10]	ZHANG Hang, HU Miaomiao, XU Yang, et al. Inhibitory effects of functionalized polycarboxylate retarder on aberrant thickening phenomena of oil well cement at high temperature[J]. Construction and Building Materials, 2021, 274: 121994.
[11]	郭鹏飞, 余燕华, 黄永毅. 不同缓凝剂的缓凝效果及其对水泥水化的影响[J]. 新型建筑材料, 2022, 49(4): 22-25.
	GUO Pengfei, YU Yanhua, HUANG Yongyi. The retarding effect of different retarders and their influence on cement hydration[J]. New Building Materials, 2022, 49(4): 22-25.
[12]	WANG Yunqing, ZOU Yiwei, TIAN Ye. Laboratory study on a large temperature difference retarder CRT601 for cementing[J]. Technology Vision, 2021, 362(32): 8-9.
[13]	赵莹, 梁骁男, 于小荣, 等. 缓凝剂ZLC的合成及应用[J]. 精细石油化工进展, 2015, 16(6): 9-11.
	ZHAO Ying, LIANG Xiaonan, YU Xiaorong, et al. Synthesis and application of retarder ZLC[J]. Advances in Fine Petrochemicals, 2015, 16(6): 9-11.
[14]	刘雪佳. 双羧基配位超分子中的配位及非键作用[D]. 天津: 天津大学, 2010.
	LIU Xuejia. Coordination and non-bonding in dicarboxyl coordination supramolecular[D]. Tianjin: Tianjin University, 2010.
[15]	ZHANG Liang, ZHUANG Jia, LIU Hanbin, et al. Terpolymerization and performance of 2-acrylamide-2-methyl propane sulfonic acid/itaconic acid/N-vinyl-2-pyrrolidone[J]. Journal of Applied Polymer Science, 2010, 117(5): 2951-2957.
[16]	李均星, 郭锦棠, 张弛, 等. 一种新型缓凝剂的制备及其在水泥基复合材料中的应用[J]. 化工进展, 2019, 38(6): 2953-2960.
	LI Junxing, GUO Jintang, ZHANG Chi, et al. Synthesis of a novel retarder and its application in cement matrix composites[J]. Chemical Industry and Engineering Progress, 2019, 38(6): 2953-2960.
[17]	彭志刚, 张博建, 冯茜, 等. 聚合物插层蒙脱土复合型高温缓凝剂的制备及性能[J]. 硅酸盐学报, 2018, 46(8): 1087-1094.
	PENG Zhigang, ZHANG Bojian, FENG Qian, et al. Preparation and performance of polymer intercalated montmorillonite composites for high-temperature retarder[J]. Journal of the Chinese Ceramic Society, 2018, 46(8): 1087-1094.
[18]	MA Cong, BU Yuhuan, CHEN Bing. Preparation and performance of a lignosulfonate-AMPS-itaconic acid graft copolymer as retarder for modified phosphoaluminate cement[J]. Construction and Building Materials, 2014, 60: 25-32.
[19]	JOSEFA Fernández, FERNANDO González, CARMEN Pesquera, et al. Qualitative and quantitative characterization of a coal power plant waste by TG/DSC/MS, XRF and XRD[J]. Journal of Thermal Analysis and Calorimetry, 2016, 125(2): 703-710.
[20]	QUERCIA G, BROUWERS H. J. H, GARNIER A,et al. Influence of olivine nano-silica on hydration and performance of oil-well cement slurries[J]. Materials & Design, 2016, 96: 162-170.
[21]	Krakowiak KONRAD J., Thomas JEFFREY J., SIMONE Musso, et al. Nano-chemo-mechanical signature of conventional oil-well cement systems: Effects of elevated temperature and curing time[J]. Cement and Concrete Research, 2015, 67: 103-121.

编号	A	B	C	D	稠化时间/min
1	79%-15%-6%	5%	30	70	174
2	79%-15%-6%	6%	45	80	170
3	79%-15%-6%	7%	60	70~80	168
4	76%-16%-8%	5%	45	70~80	185
5	76%-16%-8%	6%	60	70	178
6	76%-16%-8%	7%	30	80	182
7	73%-17%-10%	5%	60	80	180
8	73%-17%-10%	6%	30	70~80	199
9	73%-17%-10%	7%	45	70	192
K₁	171	180	185	181
K₂	182	182	182	177
K₃	190	181	175	184
R	19	2	10	7
最佳水平	A₃	B₂	C₁	D₃

编号	A	B	C	D	稠化时间/min
1	79%-15%-6%	5%	30	70	174
2	79%-15%-6%	6%	45	80	170
3	79%-15%-6%	7%	60	70~80	168
4	76%-16%-8%	5%	45	70~80	185
5	76%-16%-8%	6%	60	70	178
6	76%-16%-8%	7%	30	80	182
7	73%-17%-10%	5%	60	80	180
8	73%-17%-10%	6%	30	70~80	199
9	73%-17%-10%	7%	45	70	192
K₁	171	180	185	181
K₂	182	182	182	177
K₃	190	181	175	184
R	19	2	10	7
最佳水平	A₃	B₂	C₁	D₃

稠化温度/℃	缓凝剂加量w	初始稠度/BC	过渡时间/min	稠化时间/min
140	5%	23	10	335
160	5%	22	7	256
180	5%	20	3	199
180	5%+0.5%PS	17	3	260
160	5%+0.5%PS	16	8	316
140	5%+0.5%PS	18	10	396

稠化温度/℃	缓凝剂加量w	初始稠度/BC	过渡时间/min	稠化时间/min
140	5%	23	10	335
160	5%	22	7	256
180	5%	20	3	199
180	5%+0.5%PS	17	3	260
160	5%+0.5%PS	16	8	316
140	5%+0.5%PS	18	10	396

缓凝剂加量/%	流动度/cm	六速旋转黏度计读数						n	k/Pa∙s ⁿ
缓凝剂加量/%	流动度/cm	θ₆₀₀	θ₃₀₀	θ₂₀₀	θ₁₀₀	θ₆	θ₃	n	k/Pa∙s ⁿ
0	20.5	201.2	112.1	73.3	34.7	1.6	0.7	1.07	0.07
3	23	313.0	184.2	119.1	61.9	3.5	1.8	0.99	0.19
5	24	513.6	325.3	243.0	121.5	10.1	4.9	0.90	0.62
5+0.5PS	26	367.1	209.1	141.6	76.1	5.0	2.6	0.92	0.34