CN101864285A - Deepwater cementing low-temperature early strength agent - Google Patents

Deepwater cementing low-temperature early strength agent Download PDF

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CN101864285A
CN101864285A CN 201010200729 CN201010200729A CN101864285A CN 101864285 A CN101864285 A CN 101864285A CN 201010200729 CN201010200729 CN 201010200729 CN 201010200729 A CN201010200729 A CN 201010200729A CN 101864285 A CN101864285 A CN 101864285A
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early strength
strength agent
temperature
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CN101864285B (en
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徐璧华
宋茂林
谢应权
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Southwest Petroleum University
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Abstract

The invention relates to a deepwater cementing low-temperature early strength agent. The low-temperature early strength agent comprises the following components in percentage by weight: 33 to 66 percent of alkali metal bromides, 6 to 16 percent of sodium metaaluminate, 15 to 35 percent of alkali metal hydroxides, 8 to 15 percent of silicon dioxide and 0.8 to 1.5 percent of alcamines organics, wherein the alkali metal bromides are a mixture of one, two or more of NaBr, KBr and LiBr; the alkali metal hydroxides are NaOH, KOH or a mixture of the NaOH and KOH; and the alcamines organics are triethanolamine, triisopropanolamine or a mixture of the triethanolamine and triisopropanolamine. The deepwater cementing low-temperature early strength agent has small influence on rheological behaviour of cement paste at low temperature, can prompt the cement paste to be solidified rapidly at low temperature and reach higher early strength, shortens the thickening time of the cement paste at lower temperature and can well meet the requirements of the cementing construction of a surface casing under the conditions of low temperature, shallow gas and the like.

Description

Deepwater cementing low-temperature early strength agent
Affiliated technical field
The present invention relates to a kind of deep water cementing low-temperature early strength agent, belong to the oil gas well cementing operation technical field.
Background technology
The exploratory development of ballow hydrocarbon resources is limited by abominable complex environment and storage characteristics, has " four height " characteristics, i.e. new and high technology, excessive risk, high skill people, high repayment.Can and can a bite well exploit the time of decades safely, economically, and the test that withstand well stimulation, perforation, exploitation and the every workover treatment in process of production of oil gas well, and this is often closely related with the quality of well cementation.For the difficulty that deep-water exploration faced, often high especially to the deep water cementing specification of quality.Deep water cementing is compared with conventional cementing, and particularly top layer section well cementation often is faced with unfavorable factors such as low temperature, weak formation, shallow seated groundwater air-flow.
The water-soluble class hardening accelerator of deepwater well cementing mortar exists hydration heat big mainly based on muriate at present, side effects such as corrosion sleeve pipe and cement; But not water-soluble class hardening accelerator can only be used to have the well site of dry mixing device again, has certain application limitation, and responsive to temperature, can only be suitable for single temperature condition.
Therefore, developing a kind of novel low-temperature early strength agent prevents the annular space channelling and improves cementing quality, not only be domestic deep water hydrocarbon well, and, in the exploitation of low temperature hydrocarbon-bearing pool, have great importance for the support that provides the necessary technical of the well cementation operating mode under the cold condition in the shallow gas etc.
Summary of the invention
The object of the present invention is to provide deepwater cementing low-temperature early strength agent, this low-temperature early strength agent can shorten the thickening time of grout under cold condition, improve the early anti pressured intension of cement stone, can be used under the cold condition being particularly suitable for deep water cementing aspect in ocean under the cold condition in the hydrocarbon-bearing pool well cementation.
For reaching above technical purpose, the invention provides following technical scheme.
Deepwater cementing low-temperature early strength agent, every kind of component and content are as follows:
Alkali metal bromide: 33~66 weight %;
Sodium metaaluminate: 6~16 weight %;
Alkali metal hydroxide: 15~35 weight %;
Silicon-dioxide: 8~15 weight %;
Alcamines organism: 0.8~1.5 weight %.
Described alkali metal bromide is a kind of, two or more mixture among NaBr, KBr, the LiBr; Described alkali metal hydroxide is NaOH, KOH or its mixture; Silicon-dioxide is nano level.
Described alcamines organism is trolamine, tri-isopropanolamine or its mixture.
Above material is commercially available.
Low-temperature early strength agent preparation of compositions method of the present invention is as follows: alkali metal bromide, sodium metaaluminate, alkali metal hydroxide, silicon-dioxide and alcamines organism are weighed up according to the above ratio; Above-mentioned substance added to mix in the mixing machine successively get final product.
Alkali metal bromide among the present invention and alcamines organism can generate complex compound with cement colloidal mineral generation chemical action, have quickened the hydrated cementitious process and have promoted the development of cement stone early strength.With the alcamines organism is example, and it contains not share electron pair, thereby it is easy to dative bond with other ion, and especially some metal ions form complex ions, thereby are good complexing agents.It is easily and the Al in the cement particle surface hydrated product in basic solution 3+, Fe 3+Plasma generates water-soluble coordination compound, therefore, generates solvable point at the cement particle surface and quickens C in the G class g cement 3A, C 2A and C 4The AF dissolution rate, and accelerate with the reaction of gypsum, calcium sulphoaluminate (ettringite AFt) growing amount increases; thereupon like this will be before the grout sclerosis, basically finish volumetric expansion, thereby can improve the compactness and the ultimate compression strength thereof of cement stone, especially improve early strength.In addition, the adding of the alkali metal hydroxide among the present invention makes Ca in the liquid phase (OH) 2The steady degree of supersaturation that is situated between improves, and can more effectively stop C 3The A aquation initial stage forms loose crystalline trend, thereby improves the compactness and the intensity of cement stone.Sodium metaaluminate among the present invention, its main component is a meta-aluminate, it mainly acts on is the alkalescence that effective component is provided and has strengthened solution for the formation of ettringite AFt with lime, simultaneously, their thermopositive reaction at the beginning of Jia Shui have improved liquidus temperature, help promoting the formation and the slurry strength development of hydrated product.The main effect of the silicon-dioxide among the present invention is the filling concrete gap between particles, and then improves the compactness of cement stone.
Compared with prior art, low-temperature early strength agent of the present invention has following beneficial effect: (1) rheology impact to grout under cold condition is very little.(2) impel grout rapid solidification under cold condition, and reach higher early strength.(3) thickening time of grout under the shortening cold condition.Therefore can satisfy the surface string needs of cementing operations under the situations such as low temperature, shallow gas well.
Description of drawings
Fig. 1 is the low-temperature early strength agent of the present invention that adds 3 weight % in the good magnificent G level oil well cement, presses water cement ratio 0.44, and the grout of being prepared is at 30 ℃, the multiviscosisty graphic representation under the 20MPa condition.
Fig. 2 is the low-temperature early strength agent of the present invention that adds 3 weight % in the good magnificent G level oil well cement, presses water cement ratio 0.44, and the grout of being prepared is at 30 ℃, the ultimate compression strength progress curve figure under the 14MPa condition.
Embodiment
In embodiments of the present invention, specialize as nothing, per-cent all is weight percentage.
Embodiment 1:
35% Potassium Bromide, 15% sodium metaaluminate, 35% potassium hydroxide, 14% silicon-dioxide, 1% alcamines organism are weighed up according to the above ratio; Potassium Bromide, sodium metaaluminate, potassium hydroxide, silicon-dioxide, the alcamines organism that weighs up added in the mixing machine successively mix, promptly get low-temperature early strength agent of the present invention " ZQ-1 ".
Embodiment 2:
30% Sodium Bromide, 30% Potassium Bromide, 7% sodium metaaluminate, 24% sodium hydroxide, 8% silicon-dioxide, 1% alcamines organism are weighed up according to the above ratio; Sodium Bromide, Potassium Bromide, sodium metaaluminate, sodium hydroxide, silicon-dioxide, the alcamines organism that weighs up added in the mixing machine successively mix, promptly get low-temperature early strength agent of the present invention " ZQ-2 ".
Embodiment 3:
53% Sodium Bromide, 12% sodium metaaluminate, 15% sodium hydroxide, 9.2% silicon-dioxide, 0.8% alcamines organism are weighed up according to the above ratio; Sodium Bromide, sodium metaaluminate, sodium hydroxide, silicon-dioxide, the alcamines organism that weighs up added in the mixing machine successively mix, promptly get low-temperature early strength agent of the present invention " ZQ-3 ".
Embodiment 4: powerful morning of low-temperature early strength agent " ZQ-2 "
Good magnificent G level oil well cement is selected in experiment for use, and water cement ratio is 0.44 neat slurry.The ultimate compression strength experiment utilizes atmospheric low-temperature water-bath maintenance test.Under different dosages, differing temps, the different curing time condition low-temperature early strength agent to good magnificent G class g cement ultimate compression strength to influence situation as shown in table 1.
By the result as can be known, under the atmospheric low-temperature condition, low-temperature early strength agent has significant early stage enhancement to conventional density neat slurry, and temperature is low more and curing time is short more, and it is high more that cement stone ultimate compression strength increases degree.
Table 1 hardening accelerator is to the influence of cement stone ultimate compression strength
Figure GDA0000022359330000041
Embodiment 5: low-temperature early strength agent " ZQ-2 " is to grout multiviscosisty performance impact
Good magnificent G level oil well cement is selected in experiment for use, and water cement ratio is 0.44 neat slurry.Measure the thickening time of grout under the differing temps.The result is as shown in table 2.As can be seen from the table, the thickening time of grout under the cold condition can be obviously shortened in the strong agent of low temperature among the present invention, and also significantly shortening of the multiviscosisty of grout " transit time ", show certain " near right angle multiviscosisty " characteristic, have good anti-channeling.
Table 2 hardening accelerator is to grout multiviscosisty Effect on Performance
Figure GDA0000022359330000042
Embodiment 6: low-temperature early strength agent " ZQ-2 " is to mortar architecture performance impact commonly used
Low-temperature early strength agent among the present invention will successfully be promoted in oil gas well cementing job as a kind of new oil well cement additive, not only will satisfy the low-temperature high-early strength characteristic, requires to have excellent compatibility with other oil well cement additive commonly used simultaneously.
Be the adaptability of low-temperature early strength agent among check the present invention, its influence of experimental analysis to multiple mortar architecture over-all properties commonly used.Table 3 and table 4 are respectively the Effect on Performance situation of low-temperature early strength agent " ZQ-2 " to LT-1A mortar architecture, JS-2 mortar architecture, comprise performances such as fluid loss, free water, thickening time and ultimate compression strength.The curing condition of ultimate compression strength experiment wherein: maintenance in the normal pressure water-bath; The experimental pressure of thickening time is 7~15MPa.
Table 3 hardening accelerator is to the influence of LT-1A mortar architecture salient features
Figure GDA0000022359330000051
Table 4 hardening accelerator is to the influence of JS-2 mortar architecture salient features
Figure GDA0000022359330000052
Analyze from table and find out, the low-temperature early strength agent among the present invention all has significant early stage enhancement to these mortar architectures, and the over-all properties Harmony of system is good, and the thickening time is easy to regulation and control, and stability, rheological and dehydration etc. are all had no adverse effects.This research experiment has also been investigated this low-temperature early strength agent to other mortar architecture commonly used early stage enhancement effect and the Other Engineering Effect on Performance situation of (comprising LT-2 mortar architecture, HS-2A mortar architecture and latex LATEX2000 mortar architecture etc.).Experimental result shows that the admixture of low-temperature early strength agent of the present invention and these mortar architectures has excellent compatibility.
Embodiment 7: the multiviscosisty performance of low-temperature early strength agent " ZQ-2 " and ultimate compression strength analysis
Fig. 1 is " ZQ-2 " low-temperature early strength agent of adding 3% in the good magnificent G level oil well cement, press water cement ratio 0.44, the grout of being prepared is at 30 ℃, the multiviscosisty graphic representation under the 20MPa condition, can obviously be found out by figure: the thickening time is 150min, and multiviscosisty transit time is 13min.Curve is " near right angle multiviscosisty ", and the explanation system has good anti-channeling.
Fig. 2 is " ZQ-2 " low-temperature early strength agent of adding 3% in the good magnificent G level oil well cement, press water cement ratio 0.44, the grout of being prepared is at 30 ℃, use the ultimate compression strength progress curve figure of ultrasonic investigation under the 14MPa condition, can draw by map analysis: in G class g cement magma, add " ZQ-2 " low-temperature early strength agent, system 6h ultimate compression strength has improved 239.52% just up to 0.842MPa than G level magma ultimate compression strength under the same terms.Can confirm thus: the ZQ-A low-temperature early strength agent has good early strength function to G level oil well cement.

Claims (5)

1. deepwater cementing low-temperature early strength agent, every kind of component and content are as follows:
Alkali metal bromide: 33~66 weight %;
Sodium metaaluminate: 6~16 weight %;
Alkali metal hydroxide: 15~35 weight %;
Silicon-dioxide: 8~15 weight %;
Alcamines organism: 0.8~1.5 weight %.
2. low-temperature early strength agent as claimed in claim 1, it is characterized in that, described alkali metal bromide is a kind of, two or more mixture among NaBr, KBr, the LiBr, described alkali metal hydroxide is NaOH, KOH or its mixture, and described alcamines organism is trolamine, tri-isopropanolamine or its mixture.
3. low-temperature early strength agent as claimed in claim 2 is characterized in that, its component and ratio are as follows: Potassium Bromide 35 weight %, sodium metaaluminate 15 weight %, potassium hydroxide 35 weight %, silica 14 weight %, trolamine or tri-isopropanolamine 1 weight %.
4. low-temperature early strength agent as claimed in claim 2, it is characterized in that its component and ratio are as follows: Sodium Bromide 30 weight %, Potassium Bromide 30 weight %, sodium metaaluminate 7 weight %, sodium hydroxide 24 weight %, silicon-dioxide 8 weight %, trolamine or tri-isopropanolamine 1 weight %.
5. low-temperature early strength agent as claimed in claim 2, it is characterized in that its component and ratio are as follows: Sodium Bromide 53 weight %, sodium metaaluminate 12 weight %, sodium hydroxide 15 weight %, silicon-dioxide 9.2 weight %, trolamine or tri-isopropanolamine 0.8 weight %.
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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102126840A (en) * 2011-03-02 2011-07-20 陈子川 Low-temperature concrete early strength agent
CN102531443A (en) * 2010-12-13 2012-07-04 中联煤层气有限责任公司 Early strength agent composition and preparation method thereof, cement composition and uses of above
CN104031624A (en) * 2014-06-20 2014-09-10 西南石油大学 Preparation method of early strength agent of low-density cement slurry
CN105347716A (en) * 2015-11-24 2016-02-24 中国石油大学(华东) Dispersive chlorine-free low-temperature early-strength agent used for oil well cement and cement mortar including same
CN105462571A (en) * 2015-11-16 2016-04-06 中国石油大学(华东) Low-temperature cementing slurry system and composition thereof
CN104194752B (en) * 2014-08-01 2016-11-23 中国石油天然气集团公司 Coal bed gas well well cementation low-temperature early strength agent and containing its cement paste for well cementation
CN106348690A (en) * 2016-08-26 2017-01-25 北京建工新型建材有限责任公司 Masonry mortar for underwater acid environment
CN106365569A (en) * 2016-08-26 2017-02-01 北京建工新型建材有限责任公司 High-perturbance underwater masonry mortar
CN106365499A (en) * 2016-08-26 2017-02-01 北京建工新型建材有限责任公司 Special high-performance additive for underwater masonry mortar
CN106380135A (en) * 2016-08-26 2017-02-08 北京建工新型建材有限责任公司 Masonry mortar used in underwater alkaline environment
CN106542757A (en) * 2016-10-25 2017-03-29 中国石油集团川庆钻探工程有限公司长庆固井公司 A kind of alcamines reinforcing agent and preparation method and applications
CN106830744A (en) * 2017-01-06 2017-06-13 中国海洋石油总公司 A kind of well cementation early strength agent and preparation method thereof
CN108178597A (en) * 2017-12-18 2018-06-19 固岩科技发展有限公司 A kind of method of early-strong-fast-hard type cementitious material consolidated fill metal mine
CN109777375A (en) * 2019-04-01 2019-05-21 安徽陆海石油助剂科技有限公司 A kind of viscosity depressant for drilling fluid and its production method
CN111116082A (en) * 2020-02-27 2020-05-08 河海大学 MXene modified concrete early strength agent and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030172850A1 (en) * 2002-03-13 2003-09-18 Byong-Wa Chun Beneficiated water reducing compositions
CN101244918A (en) * 2008-03-14 2008-08-20 北京化工大学 Use method with calcium-aluminum hydrotalcite as concrete early strength agent

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030172850A1 (en) * 2002-03-13 2003-09-18 Byong-Wa Chun Beneficiated water reducing compositions
CN101244918A (en) * 2008-03-14 2008-08-20 北京化工大学 Use method with calcium-aluminum hydrotalcite as concrete early strength agent

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102531443A (en) * 2010-12-13 2012-07-04 中联煤层气有限责任公司 Early strength agent composition and preparation method thereof, cement composition and uses of above
CN102531443B (en) * 2010-12-13 2013-09-25 中联煤层气有限责任公司 Early strength agent composition and preparation method thereof, cement composition and uses of above
CN102126840A (en) * 2011-03-02 2011-07-20 陈子川 Low-temperature concrete early strength agent
CN104031624B (en) * 2014-06-20 2016-08-24 西南石油大学 A kind of preparation method of low-density cement mortar early strength agent
CN104031624A (en) * 2014-06-20 2014-09-10 西南石油大学 Preparation method of early strength agent of low-density cement slurry
CN104194752B (en) * 2014-08-01 2016-11-23 中国石油天然气集团公司 Coal bed gas well well cementation low-temperature early strength agent and containing its cement paste for well cementation
CN105462571B (en) * 2015-11-16 2018-06-29 中国石油大学(华东) A kind of low temperature well cementing mortar architecture and composition
CN105462571A (en) * 2015-11-16 2016-04-06 中国石油大学(华东) Low-temperature cementing slurry system and composition thereof
CN105347716A (en) * 2015-11-24 2016-02-24 中国石油大学(华东) Dispersive chlorine-free low-temperature early-strength agent used for oil well cement and cement mortar including same
CN106365499B (en) * 2016-08-26 2018-08-31 北京建工新型建材有限责任公司 Masonry mortar special additive under a kind of high-performance water
CN106365499A (en) * 2016-08-26 2017-02-01 北京建工新型建材有限责任公司 Special high-performance additive for underwater masonry mortar
CN106380135A (en) * 2016-08-26 2017-02-08 北京建工新型建材有限责任公司 Masonry mortar used in underwater alkaline environment
CN106365569A (en) * 2016-08-26 2017-02-01 北京建工新型建材有限责任公司 High-perturbance underwater masonry mortar
CN106348690A (en) * 2016-08-26 2017-01-25 北京建工新型建材有限责任公司 Masonry mortar for underwater acid environment
CN106542757A (en) * 2016-10-25 2017-03-29 中国石油集团川庆钻探工程有限公司长庆固井公司 A kind of alcamines reinforcing agent and preparation method and applications
CN106830744A (en) * 2017-01-06 2017-06-13 中国海洋石油总公司 A kind of well cementation early strength agent and preparation method thereof
CN106830744B (en) * 2017-01-06 2019-03-12 中国海洋石油集团有限公司 A kind of well cementation early strength agent and preparation method thereof
CN108178597A (en) * 2017-12-18 2018-06-19 固岩科技发展有限公司 A kind of method of early-strong-fast-hard type cementitious material consolidated fill metal mine
CN109777375A (en) * 2019-04-01 2019-05-21 安徽陆海石油助剂科技有限公司 A kind of viscosity depressant for drilling fluid and its production method
CN111116082A (en) * 2020-02-27 2020-05-08 河海大学 MXene modified concrete early strength agent and preparation method thereof

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