抗热老化降失水剂研究与应用

凌勇; 王其可; 肖尧; 杜滨; 许艺馨; 刘文明; 商晓阳

doi:10.12358/j.issn.1001-5620.2026.02.012

抗热老化降失水剂研究与应用

doi: 10.12358/j.issn.1001-5620.2026.02.012

1.
中国石油集团渤海钻探工程有限公司第二固井分公司, 天津300280
2.
中国石油集团渤海钻探工程有限公司, 天津300457

基金项目: 渤海钻探科技项目“高温水泥浆体系深化研究”（2024D20F）。

详细信息

作者简介:
凌勇，高级工程师，现在主要从事固井技术研究工作。电话（022）25961706；E-mail：ling_yong@cnpc.com.cn

中图分类号: TE256.6
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出版历程
- 收稿日期: 2025-09-20
- 修回日期: 2025-11-29
- 刊出日期: 2026-04-08

Research and Application of a Thermal-Resistant Fluid Loss Additive

1.
NO.2 Cementing Company, CNPC Bohai Drilling Engineering Co., Ltd., Tianjin 300280
2.
CNPC Bohai Drilling Engineering Co., Ltd., Tianjin 300457

摘要

摘要: 针对液体AMPS类降失水剂在中温存储（50～70 ℃）后引起水泥浆稠化时间的延长，影响水泥浆稠化稳定性的问题。通过自由基共聚法设计并合成了以AMPS、酰胺基单体和不饱和酸单体为主单体的系列降失水剂，优选了以AMPS、N,N-二甲基丙烯酰胺（DMAA）及丙烯酸（AA）为主单体的三元聚合物液体降失水剂P4。考察了残留单体、酰胺类单体、不饱和酸种类和抗水解剂加入对产物性能的影响，并通过中温热老化实验测试缓凝效果。结果表明：在高环境温度下，残留单体较多易引起降失水剂局部聚合，DMAA的引入显著抑制了酰胺基团的中温水解，以一元小分子不饱和羧酸为单体合成的降失水剂稠化性能稳定，抗水解剂在降失水剂热老化早期能起到抑制水解作用，长时间热老化后失效；在60 ℃下老化10、30、90 d及12个月的三元液体降失水剂P4性能稳定，综合性能满足SY/T 5504.2—2013标准要求，为高环境温度下的外加剂储存问题提供了有效的解决方案。
- 水泥浆 /
- 降失水剂 /
- 热老化 /
- 稠化时间 /
- 稳定性
Abstract: Liquid AMPS-based fluid loss additives, when stored at medium-temperatures (50– 70 ℃), cause the thickening time of a cement slurry to prolong, thereby affecting the thickening stability of the cement slurry. To solve this problem, a series of filter loss reducers were designed and synthesized via free radical copolymerization using AMPS, amide-based monomers and unsaturated acid monomers. Among the final synthesized products, the ternary copolymer fluid loss additive P4, which was synthesized using monomers including AMPS, N,N-dimethyl acrylamide (DMAA) and acrylic acid (AA), was selected as the optimal final product. The effects of residue monomers, types of amide monomers, unsaturated acids and hydrolysis inhibitors on the properties of the final product were investigated and the retarding effect of the fluid loss additive was tested via medium-temperature thermal aging experiments. The experimental results show that at elevated ambient temperatures, a high content of residue monomers tends to cause the fluid loss additive to locally polymerize, the introduction of DMAA significantly inhibit the medium-temperature hydrolysis of the amide groups, and the fluid loss additive synthesized with monobasic small-molecule unsaturated carboxylic acid exhibits stable thickening performance. The hydrolysis inhibitor can inhibit the hydrolysis of the fluid loss additive in the early stage of thermal aging, but fails after long-term of thermal aging. After aging at 60 ℃ for 10 days, 30 days, 90 days and 12 months, the liquid ternary polymer fluid loss additive P4 maintains stable performance, with its comprehensive performance satisfying the requirements of the SY/T 5504.2-2013 standard. This study provides an effective solution to the storage of additives under high ambient temperatures.
- Cement slurry /
- Fluid loss additive /
- Thermal aging /
- Thickening time /
- Stability

HTML全文

表 1 加有1%APS中温老化后的降失水剂绝对黏度

降失水剂	热老化后黏度/mPa·s	降失水剂	热老化后黏度/mPa·s
P1	44	P4	24
P2	53	P5	59
P3	73	P6	68
注：初始黏度为22 mPa·s。

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表 2 不同热老化时间对降失水剂稠化时间的影响

降失水剂	T_存放/ ℃	不同老化时间（d）下水泥浆的稠化时间/min
降失水剂	T_存放/ ℃	10	20	30	60	90
P4	23	105	104	106	106	108
P4	60	107	106	106	108	107
P5	23	112	112	113	112	114
P5	60	125	131	142	145	148
P6	23	109	109	108	111	109
P6	60	124	129	133	140	143

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表 3 加入酰胺类单体降失水剂水泥浆热老化后的稠化性能

降失水剂	T_老化/℃	不同老化时间（d）下水泥浆的稠化时间/min
降失水剂	T_老化/℃	10	30	60
P1	23	105	107	107
	50	120	126	133
	60	126	130	138
	70	130	132	141
P2	23	110	112	110
	50	123	127	133
	60	129	134	139
	70	132	140	145
P3	23	100	102	102
	50	113	120	126
	60	119	125	136
	70	122	131	142
P4	23	105	106	106
	50	104	106	105
	60	107	106	108
	70	108	106	105
P5	23	112	113	112
	50	121	135	140
	60	125	142	145
	70	129	141	148
P6	23	109	108	111
	50	122	131	140
	60	124	133	140
	70	130	141	149
注：胜潍G级水泥100% +3%降失水剂（P1～P6）+ 41%水，密度为1.90 g/cm³。

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表 4 抗水解剂对降失水剂稠化时间的影响

降失水剂	抗水解剂	T_老化/ ℃	t_稠化/h			黄变度
降失水剂	抗水解剂	T_老化/ ℃	10 d	30 d	60 d	10 d	30 d	60 d
P1	空白	60	126	130	138	+	+	++
P1	0.1%	60	122	123	138	+	+	++
P3	空白	60	119	125	136	+	++	++
P3	0.1%	60	115	120	137	+	++	++
P4	空白	60	107	106	108	－	－	－
P4	0.1%	60	108	108	107	－	－	－
P6	空白	60	124	133	140	－	+	++
P6	0.1%	60	119	130	138	－	+	++
注：胜潍G级水泥+3%降失水剂+水，密度1.90 g/cm³。其中描述黄变情况程度采用“﹢”和“－”，“+”表示轻微黄变，“++”表示中等黄变，“+++”表示重度黄变，“－”表示几乎没有黄变。

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表 5 加有不同热老化时间降失水剂P4后水泥浆的API失水量

热老化温度/℃	热老化时间/d	FL_API/mL
23	0	44
60	10	45
	30	44
	90	44

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表 6 加有不同热老化时间降失水剂P4的水泥石抗压强度

热老化温度/℃	热老化时间/d	p_{24 h}（30 ℃）/ MPa	p_{24 h}（60 ℃）/ MPa
23	0	25.2	26.8
60	10	24.5	27.0
	30	26.3	27.9
	90	25.8	27.2

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表 7 加有不同热老化时间降失水剂P4后水泥浆的流变性能

热老化温度/℃	热老化时间/d	φ₃₀₀	φ₁₀₀	PV/ mPa·s	YP/ Pa	n	K/ Pa·sⁿ
23	0	195	91	156.0	39.0	0.69	1.32
60	10	200	95	157.5	42.5	0.68	1.49
	30	202	93	163.5	38.5	0.71	1.26
	90	201	96	157.5	43.5	0.67	1.55

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表 8 掺有60 ℃热老化12个月降失水剂P4水泥浆的综合性能

热老化温度/℃	P4/ %	热老化时间/月	流动度/ cm	FL/ mL	t_稠化/ min	游离液/ %	沉降稳定性/ g·cm⁻³	p_{24 h}（60 ℃）/ MPa
23	3.0	12	25	44	108	0	0	27.1
60	3.0	6	25	44	108	0	0	26.5
60	3.0	12	25	46	106	0	0	27.3
注：胜潍G级水泥+3%降失水剂P4+水，密度为1.90 g/cm³，实验条件80 ℃、46.5 MPa、45 min。

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表 9 热老化前后掺有的5.5%降失水剂P4的水泥浆性能

水泥浆	热老化时间/月	T/ ℃	FL_API/ mL	t_稠化/ min
一级领浆	12	105	55	330
一级领浆	未热老化	105	55	325
一级尾浆	12	105	50	194
一级尾浆	未热老化	105	50	189
二级尾浆	12	76	52	177
二级尾浆	未热老化	76	52	180

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