CN102775972B - Liquid high-temperature resistant declining agent for well cementation and preparation method thereof - Google Patents
Liquid high-temperature resistant declining agent for well cementation and preparation method thereof Download PDFInfo
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- CN102775972B CN102775972B CN201210246553.6A CN201210246553A CN102775972B CN 102775972 B CN102775972 B CN 102775972B CN 201210246553 A CN201210246553 A CN 201210246553A CN 102775972 B CN102775972 B CN 102775972B
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Abstract
The invention relates to a liquid high-temperature resistant declining agent. The liquid high-temperature resistant declining agent comprises the following components: silicon powder and micro-silica powder in the mass ratio of 9:1 to 1:9, 0.1-0.5 percent of polycarboxylic acid dispersing agent based on total mass of the silicon powder and micro-silica powder, 30-40 percent of deionized water based on total mass of the silicon powder and micro-silica powder and relevant auxiliaries. The invention also relates to a method for preparing the liquid high-temperature resistant declining agent. According to the preparation method, the liquid high-temperature resistant declining agent with high solid content, low viscosity and stable storage can be manufactured, and can be used for well cementation operation of which the temperature is more than 110 DEG C, so that the intensity of cement stones is prevented from declining under high temperature.
Description
Technical field
The present invention relates to a kind of liquid high temperature resistance decline agent and preparation method thereof, particularly a kind of admixture that is applicable to the decline of cementing concrete stone high temperature resistance and preparation method thereof.
Background technology
Well cementation claims again cementing job, by the process of the annular space between grout sprue bushing and stratum.The annular space Behavior of Hardened Cement Paste forming after well cementation, its long-term integrity is technical development emphasis in the past and from now on, wherein " decline of Behavior of Hardened Cement Paste high temperature " is one of factor affecting Behavior of Hardened Cement Paste long-term integrity.(Swayze is found in early stage research, International petroleum association, 1954), in the time that temperature is greater than 110 DEG C, for silicate cement, can there is phase transition in the CSH gel that plays intensity in hydrated product, generate a kind of degree of crystallinity and the high α-C of density ratio CSH gel
2sH thing phase, declines cement strength and perviousness increases, and this phenomenon is referred to as the decline of Behavior of Hardened Cement Paste high temperature.
At present, the Behavior of Hardened Cement Paste high temperature decline problem running into for hot hole and thick oil thermal extraction, the technical measures of solution have:
One is to adopt non-silicate cement, as Sorel cement (Ashok Santra, SPE121102,2009) and phosphor aluminate cement (Crystal lynne keys, US7863224,2011).Halliburton company
and Thermalock
tMhigh-temperature cement slurry system has just adopted respectively Sorel cement and phosphor aluminate cement.
Another kind is by add extra material or material modified in silicate cement, prevents the decline of Behavior of Hardened Cement Paste high temperature.As: add 30～40% or the silica flour of high-content (silica flour) more.In the recent period, BJ company discloses the patent (Di Lullo Arias Gino F, US7448449,2011) that adds 5% bismuth oxide can prevent Behavior of Hardened Cement Paste high temperature decline at 176 DEG C in silicate cement.People (the SPE21597 such as R.Dillenbeck III, 1990) report, SILICA FUME (Silica fume, or microsilica) by consuming the calcium hydroxide in hydrolysis product of cement, contribute to the decline of Behavior of Hardened Cement Paste high temperature resistance, based on this effect add in addition the colloid silicon less than SILICA FUME, as Eka company
w-8.By mixing natural zeolite, can obtain the low-density cement mortar for geothermal well, as the VariSeal mortar architecture of Halliburton company.
In these technology, using general and proven technique is in silicate cement, to add silica flour, or adds silica flour and SILICA FUME simultaneously.This know-why is: reduce the Ca/Si ratio in Behavior of Hardened Cement Paste.Conventionally in CSH gel, Ca/Si ratio is about 1.5, and in the time that temperature is greater than 110 DEG C, CSH gel generation phase transition, generates α-C that perviousness is high, intensity is low
2sH thing phase, but when adding 30～40% silica flour can make Ca/Si ratio be less than or equal to 1, in the time that temperature is greater than 110 DEG C, form perviousness is low, intensity is high tobermorite (Tobermorite, C
5s
6h
5), in the time that temperature is greater than 150 DEG C, tobermorite thing inversion of phases is xonotlite (Xonotlite, C
6s
6and a small amount of white silicon calcium stone (Gyrolite, C H)
5s
3h
2), perviousness is slightly increased with intensity and slightly decline.In silicate cement hydration product, except rising the CSH gel of intensity, also contain 10～20% calcium hydroxide, calcium hydroxide can impel CSH gel to be at high temperature converted into α-C
2sH thing phase, adds the SILICA FUME can consume calcium hydroxide, and produces CSH gel.
Use silica flour and the SILICA FUME of powder form to have following problem:
Silica flour is the silicon-dioxide of crystal form, and SILICA FUME is the silicon-dioxide of unformed shape, and Hygiene Toxicology confirms that the silicon-dioxide of crystal form is a kind of lung carcinogens matter, and its harm to human body is larger than the silicon-dioxide of unformed shape.Before cementing operation, silica flour or and SILICA FUME elder generation and dry-mixed cement, in mixing, easily produce airborne dust, this is large to operator's damage to person, and exists and mix inhomogenous problem.For marine well cementing operation, on the one hand, due to platform cement storage tank limited amount, in the time carrying out the well cementation of hot hole section, often exist bulk cement storage tank not more than needed to deposit the situation of silica flour mixed cement, on the other hand, for unspent mixed silicon cement, often be not suitable for other well section well cementation, can only abandon unspent silica flour mixed cement, cause waste and environmental pollution.Meanwhile, transmit cement and silica flour by gas circuit, have the loss of a certain amount of cement and silica flour dust.The liquid high temperature resistance decline agent of preparing taking silica flour and SILICA FUME as raw material, can address the above problem.
Have about the preparation method of liquid high temperature resistance decline agent at present:
The people (US7393407,2008) such as Eldar O Dingsoyr disclose taking xanthan gum or carboxylic acid methyl Mierocrystalline cellulose as suspension stabilizer, and preferably xanthan gum is stablizer, prepares the waterborne suspension of silica flour and SILICA FUME.
People (the US7238733 such as Vijn Jan Pieter, 2008) disclose taking colloid carbon black or as soil or carrageenin or AMPS/NNDMA multipolymer as suspension stabilizer, prepare the waterborne suspension of silica flour and SILICA FUME, as Behavior of Hardened Cement Paste liquid high temperature resistance decline agent.
In the waterborne suspension process of preparing silica flour and SILICA FUME, find, adopt aforesaid method can not obtain well the waterborne suspension of good fluidity, stable storing, its reason is, the reasons such as a small amount of impurity of SILICA FUME water requirement greatly and in SILICA FUME.So prepare the waterborne suspension of silica flour and SILICA FUME, first need to prepare the SILICA FUME waterborne suspension of good fluidity, stable storing, consider and then the suspension problem of silica flour in waterborne suspension.US4321243 (1982), JP60129132 (1985), US4888058 (1989), JP2145417 (1990), US5176752 (1993), JP8333144 (1996), JP2002137947 (2002), JP2007161531 (2007), US7393407 (2008), JP2008037689 (2008) patent all discloses the method for preparing waterborne suspension taking SILICA FUME as raw material, according to these disclosed methods, is also difficult to obtain the SILICA FUME suspension of good fluidity, stable storing.
Summary of the invention
Order of the present invention is to provide that a kind of solid content is high, viscosity is low, the silica flour of stable storing, SILICA FUME waterborne suspension, and this waterborne suspension can be used as liquid high temperature resistance decline agent, for hot hole and thick oil thermal extraction, prevents the high temperature decline of cementing concrete stone.
Another object of the present invention is to provide the preparation method of described silicon slurry.
Liquid high temperature resistance of the present invention decline agent comprises 30～40% deionized water of 0.1～0.5% polycarboxylic acid dispersant of silica flour, SILICA FUME and the total mass based on described silica flour and SILICA FUME and the total mass based on described silica flour and SILICA FUME.
According to embodiment of the present invention, described silica flour is the silicon dioxide powder of natural siliceous sand or natural silica crystal form of gained after physics fragmentation, is preferably dioxide-containing silica and is greater than 90%, and more preferably, the size range of silica flour is 2～200 μ m.
According to embodiment of the present invention, described SILICA FUME is the amorphous silica flue dust by product of smelting ferrosilicon or metal smelting silicon gained, be preferably the flue dust that the dioxide-containing silica of metal smelting silicon gained is greater than 93%, more preferably, median particle diameter (D50) the < 0.3 μ m of described SILICA FUME, the oxide contents such as calcium, iron, magnesium are less than 5%.
According to embodiment of the present invention, the mass ratio of described silica flour and SILICA FUME is 9: 1～1: 9, is preferably 7: 3.
According to technical scheme of the present invention, described polycarboxylic acid dispersant is the polycarboxylic acid dispersant containing polyether lateral chain, its molecular characterization is: the block forming taking polyoxyethylene segment or polyoxyethylene and polyoxypropylene is as side chain, the group that contains carboxylic acid group on main chain or also contain the cloudy lotus property such as sulfonic group, the pectination molecular structure forming with this.
According to embodiment of the present invention, described liquid high temperature resistance decline agent also comprises at least one in following auxiliary agent: 0.1～0.3% anticorrosion and bactericidal agent of 0.1～0.5% stablizer of the total mass based on described silica flour, SILICA FUME, the total mass based on described silica flour, SILICA FUME.Wherein said stablizer can be warm human relations glue; Described anticorrosion and bactericidal agent can be isothiazolinone.
The preparation method of liquid high temperature resistance of the present invention decline agent comprises the steps: to add 0.1～0.5% the polycarboxylic acid dispersant based on described silica flour and SILICA FUME total mass in 30～40% deionized water of the total mass based on silica flour and SILICA FUME, stirs; Then under high-speed stirring, add described silica flour and SILICA FUME, stir.
According to embodiment of the present invention, the preparation method of described liquid high temperature resistance decline agent also comprises: dissolve 0.1～0.5% the stablizer based on silica flour and SILICA FUME total mass with 1/50 of the total Water of described deionized water in advance, after fully dissolving, placement is spent the night; In remaining described deionized water, add described polycarboxylic acid dispersant again, stir; Then under high-speed stirring, add described silica flour and SILICA FUME, high-speed stirring is after 1 hour, then adds the stabiliser solution fully dissolving in advance, and stirring at low speed evenly.
According to embodiment of the present invention, the preparation method of described liquid high temperature resistance decline agent further comprises: add described polycarboxylic acid dispersant in described deionized water in, add 0.1～0.3% the anticorrosion and bactericidal agent based on silica flour and SILICA FUME total mass.
In above-mentioned preparation method, high-speed stirring speed can be 4000～8000rpm, and stirring at low speed speed can be and is less than 1000rpm.
According to embodiment of the present invention, in above-mentioned preparation method, described silica flour is the silicon dioxide powder of natural siliceous sand or natural silica crystal form of gained after physics fragmentation, is preferably dioxide-containing silica and is greater than 90%, more preferably, the size range of silica flour is 2～200 μ m; Described SILICA FUME is the amorphous silica flue dust by product of smelting ferrosilicon or metal smelting silicon gained, be preferably the flue dust that the dioxide-containing silica of metal smelting silicon gained is greater than 93%, more preferably, median particle diameter (D50) the < 0.3 μ m of described SILICA FUME, the oxide contents such as calcium, iron, magnesium are less than 5%; The mass ratio of described silica flour and SILICA FUME is 9: 1～1: 9, is preferably 7: 3.
In liquid high temperature resistance decline agent preparation method of the present invention, the each auxiliary agent adopting is described as follows:
1. dispersion agent: be polycarboxylic acid dispersant, preferably contain the polycarboxylic acid dispersant of polyether lateral chain, its molecular structure is that the block that forms taking polyoxyethylene segment or polyoxyethylene and polyoxypropylene is as side chain, the group that contains carboxylic acid group on main chain or also contain the cloudy lotus property such as sulfonic group, and the pectination molecular structure forming.As adopted
series water reducer (German BASF AG product), as
fS10,
fS20,
fS30,
fS40,
fS60,
fW10, or
series water reducer (German BASF AG product), as
1641,
2641,
2651, or
coating dispersant, as
2450,
3400,
3440.Be preferably
fS20 and
4343, its dosage is 0.1～0.5%, is further optimized for 0.3～0.45%;
2. stablizer: for synthetic or water-soluble polymer, as AMPS/NNDMA multipolymer, derivatived cellulose, biological polymer etc.Be preferably warm human relations glue, its dosage is 0.1～0.5%;
3. anticorrosion and bactericidal agent: be aldehydes, isothiazolinone, benzothiazole quinoline class, organic bromine class, quaternary ammonium salt or chloride anticorrosion and bactericidal agent etc., be preferably isothiazolinone, as K2F (Beijing Orient Ao Han chemical company), its dosage is 0.1～0.3%;
Brief description of the drawings
Fig. 1 is under 165 DEG C of conditions, ultrasonic investigation strength of cement grout progress curve figure.
Fig. 2 is under 127 DEG C of conditions, ultrasonic investigation strength of cement grout progress curve figure.
Embodiment
The present invention is described in further detail below, so that those skilled in the art can put into practice the present invention.Should be appreciated that and can adopt other embodiments, and can make suitable change and not depart from the spirit or scope of the present invention.For fear of for making those skilled in the art can put into practice unnecessary details the present invention, specification sheets may omit some known to those skilled in the art information.Therefore, below describe in detail and should not understand with restrictive meaning, and scope of the present invention is only defined by claims.
The ratio of mentioning herein, as not specified (NS), is mass ratio.
Embodiment 1
Take 40% the deionized water based on silica flour and SILICA FUME total mass, dissolve 0.15% the warm human relations gum stabilizing agents based on silica flour and SILICA FUME total mass in advance with 1/50 of total Water, dissolving is spent the night.Residue water is added in the container with high speed agitator, and add based on 0.30% of silica flour and SILICA FUME total mass
fS20 dispersion agent, stirs.Then under high-speed stirring, (can be 4000～8000rpm) and slowly add mass ratio and be 3/7 SILICA FUME and silica flour, after high-speed stirring 1 hour, stirring at low speed (can be and be less than 1000rpm) adds the warm human relations gum stabilizing agents dissolving in advance, the liquid high temperature resistance decline agent A that gets final product describedly.Equally, according to table 1, also can prepare liquid high temperature resistance decline agent B and C, prepared liquid high temperature resistance decline agent rheological and stability in storage evaluation result are in table 1.
The evaluation result of table 1 liquid high temperature resistance stablizer
Note: " * " represents on-the-spot mud evaluation (water-base drilling fluid, the second edition) standard test according to ISO10414-1:2008; "/" can be recovered flow state after representing to stir;
sF20 is water reducer (German BASF AG);
4343 is coating dispersant (German BASF AG); K2F is isothiazolinone anticorrosion and bactericidal agent (Beijing Orient Ao Han chemical company).
Embodiment 2
Adopt U.S. Chandler ultrasonic intensity instrument, follow the tracks of each grout strength development situation in long-term maintenance processes.Result as shown in Figures 1 and 2.
Accompanying drawing 1 and accompanying drawing 2 are illustrated respectively under 165 DEG C and 127 DEG C of High Temperature Curings, do not add high temperature resistance decline agent grout C, add 35% (by cement quality) silica flour grout B and add the strength development trend of the grout A of the liquid high temperature resistance decline agent of preparing according to the application.The test condition of accompanying drawing 1 and accompanying drawing 2 is respectively: 165 DEG C, and 21Mpa; 127 DEG C, 21Mpa.
The dispensing information of A, B, C grout is as follows:
A grout formula: G class g cement 100%+PC-G80L 3%+PC-F40L 2%+PC-X60L 1%+ fresh water 44%+A liquid high temperature resistance decline agent 41%
B grout formula: G class g cement 100%+PC-G80L 3%+PC-F40L 2%+PC-X60L 1%+ fresh water 44%+PC-C8135%
C grout formula: G class g cement 100%+PC-G80L 3%+PC-F40L 2%+PC-X60L 1%+ fresh water 44%
In above-mentioned formula, PC-G80L is AMPS polymer class well cementation water retaining (Tianjin CNOOC takes chemical company's product); PC-F40L is sulfonation condensation class well cementation dispersion agent (Tianjin CNOOC takes chemical company's product); PC-X601L is phosphoric acid ester well cementation defoamer (Tianjin CNOOC takes chemical company's product); PC-C81 is 200 order silica flours (Tianjin CNOOC takes chemical company's product).
Result shows, do not add the grout of silica flour or high temperature resistance decline agent, in 24 hours strength retrogression very obvious, explanation simultaneously, the liquid high temperature resistance decline agent of preparing according to the disclosed method of the application can substitute silica flour, for preventing the generation of decay.And under 165 DEG C of hot conditionss, liquid high temperature resistance decline agent of the present invention prevents that the effect of strength of cement grout decline is better than silica flour.
In sum; these are only preferred embodiment of the present invention, be not intended to limit protection scope of the present invention, therefore; all any amendments of doing within the spirit and principles in the present invention, be equal to replacement, improvement etc., within protection scope of the present invention all should be included in.
Claims (7)
1. a liquid high temperature resistance decline agent, it is by 30～40% deionized water of 0.1～0.5% polycarboxylic acid dispersant of silica flour, SILICA FUME, total mass based on described silica flour and SILICA FUME and the total mass based on described silica flour and SILICA FUME, and 0.1～0.5% warm human relations glue of total mass based on described silica flour, SILICA FUME and/or 0.1～0.3% anticorrosion and bactericidal agent composition.
2. liquid high temperature resistance as claimed in claim 1 decline agent, wherein said silica flour is the silicon dioxide powder of natural siliceous sand or natural silica crystal form of gained after physics fragmentation, dioxide-containing silica is greater than 90%, size range is 2～200 μ m.
3. liquid high temperature resistance decline agent as claimed in claim 1, wherein said SILICA FUME is the amorphous silica flue dust of smelting ferrosilicon or metal smelting silicon gained, dioxide-containing silica is greater than 93%, median particle diameter <0.3 μ m, the oxide contents such as calcium, iron, magnesium are less than 5%.
4. the decline of the liquid high temperature resistance as described in any one in claim 1-3 agent, the mass ratio of wherein said silica flour, SILICA FUME is 9:1～1:9.
5. the decline of the liquid high temperature resistance as described in any one in claim 1-3 agent, wherein said polycarboxylic acid dispersant is the polycarboxylic acid dispersant containing polyether lateral chain, its molecular characterization is: the block forming taking polyoxyethylene segment or polyoxyethylene and polyoxypropylene is as side chain, on main chain, contain the group of cloudy lotus property, the pectination molecular structure forming with this.
6. liquid high temperature resistance decline agent as claimed in claim 1, wherein said anticorrosion and bactericidal agent is isothiazolinone.
7. a method of preparing the liquid high temperature resistance decline agent as described in any one in claim 1-6, it comprises the following steps:
In 30～40% deionized water of the total mass based on silica flour and SILICA FUME, add 0.1～0.5% the polycarboxylic acid dispersant based on described silica flour and SILICA FUME total mass, stir; Then under high-speed stirring, add described silica flour and SILICA FUME, stir, described method also comprises:
Dissolve 0.1～0.5% the warm human relations glue based on silica flour and SILICA FUME total mass with 1/50 of the total Water of described deionized water in advance, after fully dissolving, place and spend the night, and after described silica flour and SILICA FUME, adding the warm human relations sol solution fully dissolving in advance adding, stirring at low speed is even; And/or
Add described polycarboxylic acid dispersant in described deionized water in, add 0.1～0.3% the anticorrosion and bactericidal agent based on silica flour and SILICA FUME total mass.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103694975A (en) * | 2013-12-31 | 2014-04-02 | 中国海洋石油总公司 | Cement paste stabilizer and preparation method thereof |
| CN105567191B (en) * | 2014-10-13 | 2018-09-25 | 中国石油化工股份有限公司 | A kind of micro- silicon suspension of Weak Gels, preparation method and application |
| CN105505351B (en) * | 2014-10-14 | 2018-07-27 | 中国石油化工股份有限公司 | Free hydraulic control preparation of a kind of cementing slurry and the preparation method and application thereof |
| CN105567195B (en) * | 2014-10-14 | 2018-07-27 | 中国石油化工股份有限公司 | Free hydraulic control preparation of a kind of cementing slurry and the preparation method and application thereof |
| CN105176505B (en) * | 2015-06-15 | 2017-12-05 | 中国石油天然气集团公司 | A kind of cement paste for well cementation stabilizer and preparation method and application |
| CN105255462B (en) * | 2015-09-02 | 2019-02-12 | 南京云越新材料科技有限公司 | A kind of liquid silicon and preparation method thereof |
| CN105295875A (en) * | 2015-10-01 | 2016-02-03 | 中国石油集团西部钻探工程有限公司 | Heat insulation cement paste and preparation method thereof |
| CN107200493A (en) * | 2017-06-28 | 2017-09-26 | 四川宏升石油技术开发有限责任公司 | Oil well cement high temperature intensity stabilization agent |
| CN110484223B (en) * | 2018-05-15 | 2021-09-21 | 中国石油化工股份有限公司 | Oil well cement slurry system for preventing high-temperature strength from declining and preparation method thereof |
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| WO2012015308A1 (en) * | 2010-07-26 | 2012-02-02 | Elkem As | Aqueous slurry of amorphous silica and method for its production |
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| US20030181542A1 (en) * | 2002-03-21 | 2003-09-25 | Vijn Jan Pieter | Storable water-silica suspensions and methods |
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| JP2002137947A (en) * | 2000-10-27 | 2002-05-14 | Sumitomo Osaka Cement Co Ltd | Silica fume slurry for admixing cement |
| WO2012015308A1 (en) * | 2010-07-26 | 2012-02-02 | Elkem As | Aqueous slurry of amorphous silica and method for its production |
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