CN105505351B - Free hydraulic control preparation of a kind of cementing slurry and the preparation method and application thereof - Google Patents
Free hydraulic control preparation of a kind of cementing slurry and the preparation method and application thereof Download PDFInfo
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- CN105505351B CN105505351B CN201410541297.2A CN201410541297A CN105505351B CN 105505351 B CN105505351 B CN 105505351B CN 201410541297 A CN201410541297 A CN 201410541297A CN 105505351 B CN105505351 B CN 105505351B
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Abstract
The present invention relates to free hydraulic control preparations of a kind of cementing slurry in oil gas well cementing operation field and the preparation method and application thereof.The present invention a kind of cementing slurry use free hydraulic control preparation, for include blending following components suspension：Nanometer attapulgite, nano silicon dioxide, dispersant, slurry stabilizer and water；Wherein the parts by weight of water are 100 parts；The nanometer attapulgite, 10~30 parts；The nano silicon dioxide, 20~40 parts；The dispersant is selected from least one of polycarboxylate dispersant, silane copolymer dispersant or polysulfonate acid dispersant, 0.1~1 part；The slurry stabilizer is selected from hydroxyethyl cellulose, sodium carboxymethylcellulose, xanthans, scleroglucan, at least one of welan gum, 0.5~1 part.By using the free hydraulic control preparation of cementing slurry of the present invention, the free liquid of cementing slurry can be effectively eliminated or reduce, convenient for the preparation of zero free liquid cement mortar of well cementation.
Description
Technical field
The present invention relates to the free hydraulic control preparations of the cement mortar in oil gas well cementing operation field, furtherly, are related to a kind of solid
Free hydraulic control preparation of cementing slurry for well and the preparation method and application thereof.
Background technology
When diameter segment is cemented the well, in annular space concrete column, larger particle can settle under gravity, Ke Nengyou
The tendency of aggregation and bridge plug, and the free liquid in position below bridge plug just produces sink or water band when being populated with, when pressurization, cause
Behavior of Hardened Cement Paste ruptures.In addition to this, free liquid, which is assembled, to form water pocket and also interferes cement to the cementing of casing and stratum.It may also be too early
Ground is gelled, and generates lower static pressure to stratum or does not generate static pressure, and has channeling occurs.In horizontal cementing, what horizontal segment was formed
Free liquid can be moved up gradually, and when reaching a certain amount of, the free liquid capsule on annular space cement top is interconnected, and constitutes free liquid bath
Or water band, has channeling is also easily led to, cementing quality is influenced.
At present mainly there is the additive of the free liquid of control in well cementation：Bentonite, attapulgite, sodium metasilicate, diatomite, water
Glass, natural volcanic ash, flyash, alum or aluminum sulfate, cellulose, aluminium chloride, superfine cement etc., but its function and effect
There is certain limitation.Such as bentonite, attapulgite, the free liquid effect unobvious of diatomite control and influence Behavior of Hardened Cement Paste are strong
Degree；Superfine cement hydration rate is too fast, and there are uncertainties；Sodium metasilicate, waterglass are used frequently as early strength agent, and dosage becomes
Change can influence cement paste rheological matter, control free liquid effect unobvious；Alum or aluminum sulfate, cellulose, aluminium chloride etc.
Easily cement mortar is made to thicken.The control for not being fully solved free liquid in well cementation is used alone in the above additive or extra material
Problem stablizes ripe free hydraulic control preparation without being formed.
Qiu it is mediate and etc. describe liquid silicon and can reduce the free liquid of cement mortar.(Qiu Xiehe, Wang Liangcai, Guo Guangping
.Microblock the evaluation of liquid silicon and application [J] Drilling and completion fluids .2010 (04) in Chinese oil field) wherein introduce
Liquid silicon is used as free hydraulic control preparation, has obvious effects on, but the dosage of the technical solution liquid silicon is larger, general addition 10% with
On.
Invention content
In order to solve above-mentioned technical problem of the existing technology, the present invention provides a kind of free liquid of cementing slurry
Controlling agent and the preparation method and application thereof, convenient for the preparation of zero free liquid cement mortar of well cementation, preparation method is simple, at low cost
It is honest and clean, and using effect is good, and usage amount is few.
One of the object of the invention is to provide a kind of free hydraulic control preparation of cementing slurry, to include blending with the following group
The suspension divided：Nanometer attapulgite (also known as palygorskite or attapulgite), nano silicon dioxide, dispersant, slurry stabilizer
And water, form suspended liquid；Wherein, in terms of parts by weight, the parts by weight of water are 100 parts；The nanometer attapulgite, grain size
5~200nm, dosage are 10~30 parts, preferably 20~30 parts；The nano silicon dioxide, 10~260nm of grain size, dosage 20
~40 parts, preferably 20~30 parts.The dosage of the dispersant is 0.1~1 part, preferably 0.5~0.7 part, specific optional autohemagglutination carboxylic
At least one of acid dispersant, silane copolymer dispersant or polysulfonate acid dispersant；The dosage of the slurry stabilizer be 0.5~
1 part (preferably 0.5~0.6 part), in hydroxyethyl cellulose, sodium carboxymethylcellulose, xanthans, scleroglucan, welan gum
At least one.Wherein, nanometer attapulgite and nano silicon dioxide primarily serve the effect of control Free water, and with dispersant
Suspended liquid is prepared into convenient for scene use with slurry, facilitates its application.Meanwhile it is long-term convenient for product that paddle body stabilizer is added
Storage prevents its precipitation, increases stability.
Wherein, the polycarboxylate dispersant can be selected from polyacrylic acid, maleic acid-acrylic acid copolymer, acrylic acid-acrylic acid
Hydroxypropyl ester copolymer, acrylic acid-acrylic ester-phosphonic acids-co-polymer of sulfonate, acrylic acid-acrylic ester-co-polymer of sulfonate,
At least one of styrene-maleic anhydride copolymer, wherein preferred polyacrylic acid；The silane copolymer dispersant can be selected from
Polyether-modified Dimethicone Copolyol body, end group carry hydrolyzable silane key-Si (- O-CH3)3Polymer in extremely
Few one kind, wherein preferred, polyethers modified dimethyl polysiloxane copolymer；The polysulfonate acid dispersant can be selected from acrylic acid -2-
At least one of acrylamide-2-methyl propane sulfonic copolymer, sodium pyrosulfite-formaldehyde-acetone copolymer, wherein preferably
Sodium pyrosulfite-formaldehyde-acetone copolymer.
In order to further enhance product extended storage stability, prevent its precipitation, cementing slurry of the present invention from using certainly
PH value by hydraulic control preparation is preferably 9~11.
The two of the object of the invention are to provide a kind of preparation method of the free hydraulic control preparation of cementing slurry, including following step
Suddenly：
To include that component including component described above is mixed into suspension to get well cementation water of the present invention
The free hydraulic control preparation of mud.Wherein, the pH value of the suspension is preferably adjusted to 9~11.
The three of the object of the invention are cementing slurry application of the free hydraulic control preparation in cement mortar, especially
Application in cementing slurry.
Application of the cementing slurry with free hydraulic control preparation in cement mortar, including the cementing slurry is used certainly
Cement mortar is made by hydraulic control preparation and cement and cement mortar institute adding assistant etc. after mixing；It is made into institute's adding assistant of cement mortar,
Such as antifoaming agent, fluid loss agent etc., and the step of being made into cement mortar and equipment are existing in the prior art.
The wherein described cementing slurry is the 1~5% of cement weight with the dosage of free hydraulic control preparation.
The above mixing can be various hybrid modes in the prior art, such as stirring etc., and device therefor can be
Various mixing apparatus in the prior art, such as blender etc..
By using the free hydraulic control preparation of cementing slurry of the present invention, cementing slurry can be improved and control free liquid
Performance, and the free liquid of cementing slurry can be effectively eliminated or reduce, convenient for the preparation of zero free liquid cement mortar of well cementation, and make
Good with effect, usage amount is few, has preferable promotion and application value.
Specific implementation mode
With reference to embodiment, further illustrate the present invention.
Raw materials used source：
Nanometer attapulgite：Changzhou Jiuchuan Nano Material Technology Co., Ltd., high-purity Nano-class attapulgite clay；
Nano silicon dioxide：Haitai Nano Material Co., Ltd., Nanjing, nano silicon oxide；
Polycarboxylate dispersant：Dezhou continental shelf petroleum works Technology Co., Ltd., DZH-1；
Polysulfonate acid dispersant：Dezhou continental shelf petroleum works Technology Co., Ltd., DZS；
Silane copolymer dispersant：Hess steps functional material (Shanghai) Co., Ltd., Hydispex P104S；
Slurry stabilizer hydroxyethyl cellulose：Changzhou Kai Jie Chemical Co., Ltd.s, hydroxyethyl cellulose；
Slurry stabilizer xanthans：Zibo Deosen Biochemical Ltd., BP9260；
Slurry stabilizer welan gum：U.S. Si Bikai can company, KELCO-DG-F diutans；
Slurry stabilizer scleroglucan：French Sanofi Industrie companies, Actigum CS-11；
NaOH：Commercial product；
Oil-well cement：Sichuan Jiahua Enterprise (Group) Corp., Ltd. praises China's G-level high oil-resistant well cement；
Water：General tap water；
Antifoaming agent：Dezhou continental shelf petroleum works Technology Co., Ltd., DZX；
Fluid loss agent：Dezhou continental shelf petroleum works Technology Co., Ltd., DZJY；
Other reagents are commercial product.
One, prepared by free hydraulic control preparation
Embodiment 1
It is as follows using raw material：
The dosage of water is 100g；
Nanometer attapulgite, 20~50nm of grain size, dosage 20g；
Nano silicon dioxide, 30~100nm of grain size, dosage 30g；
Polycarboxylate dispersant's dosage is 0.5g；
Slurry stabilizer hydroxyethyl cellulose dosage is 0.5g；
Preparation method：Said components are mixed, high speed (12000 ± 500 revs/min) stirs evenly, and NaOH adjusts suspension
PH=9 is to get the free hydraulic control preparation of cementing slurry of the invention.
Embodiment 2
It is as follows using raw material：
The dosage of water is 100g；
Nanometer attapulgite, 10~20nm of grain size, dosage 10g；
Nano silicon dioxide, 20~50nm of grain size, dosage 30g；
Silane copolymer dispersant dosage is 1g；
Slurry stabilizer xanthans dosage is 0.5g；
Preparation method：Said components are mixed, high speed (12000 ± 500 revs/min) stirs evenly, and NaOH adjusts suspension
PH=10 is to get the free hydraulic control preparation of cementing slurry of the invention.
Embodiment 3
It is as follows using raw material：
The dosage of water is 100g；
Nanometer attapulgite, 30~100nm of grain size, dosage 30g；
Nano silicon dioxide, 100~200nm of grain size, dosage 30g；
Silane copolymer dispersant dosage is 0.5g；
Slurry stabilizer welan gum dosage is 0.5g；
Preparation method：Said components are mixed, high speed (12000 ± 500 revs/min) stirs evenly, and NaOH adjusts suspension
PH=9 is to get the free hydraulic control preparation of cementing slurry of the invention.
Embodiment 4
It is as follows using raw material：
The dosage of water is 100g；
Nanometer attapulgite, 100~200nm of grain size, dosage 30g；
Nano silicon dioxide, 200~260nm of grain size, dosage 30g；
Silane copolymer dispersant dosage is 0.2g；
Slurry stabilizer scleroglucan dosage is 0.6g；
Preparation method：Said components are mixed, high speed (12000 ± 500 revs/min) stirs evenly, and NaOH adjusts suspension
PH=11 is to get the free hydraulic control preparation of cementing slurry of the invention.
Embodiment 5
It is as follows using raw material：
The dosage of water is 100g；
Nanometer attapulgite, 100~200nm of grain size, dosage 20g；
Nano silicon dioxide, 10~30nm of grain size, dosage 40g；
Polysulfonate acid dispersant dosage is 0.1g；
Slurry stabilizer sodium carboxymethylcellulose dosage is 1g；
Preparation method：Said components are mixed, high speed (12000 ± 500 revs/min) stirs evenly, and NaOH adjusts suspension
PH=10 is to get the free hydraulic control preparation of cementing slurry of the invention.
Embodiment 6
It is as follows using raw material：
The dosage of water is 100g；
Nanometer attapulgite, 5~10nm of grain size, dosage 30g；
Nano silicon dioxide, 200~260nm of grain size, dosage 20g；
Silane copolymer dispersant dosage is 0.7g；
Slurry stabilizer scleroglucan dosage is 0.8g；
Preparation method：Said components are mixed, high speed (12000 ± 500 revs/min) stirs evenly, and NaOH adjusts suspension
PH=11 is to get the free hydraulic control preparation of cementing slurry of the invention.
Two, free liquid test
1, prepared by blank cement mortar
Weigh 500g oil-well cements, 215g water, 0.5g antifoaming agent, 5g fluid loss agents.Water, fluid loss agent and antifoaming agent are put
In the mixing container, blender is with (4000 ± 200 revs/min) rotations of low speed, and the cement weighed is added in 15 seconds, covers and stirs
The lid of device is mixed, and continues stirring 35 seconds under high speed (12000 ± 500 revs/min), blank cement mortar is made.
2, comparative example 1
It is prepared by " aluminium chloride " cement mortar
Weigh 500g oil-well cements, 215g water, 0.5g antifoaming agent, 5g fluid loss agents, 2.5g aluminium chlorides.By oil well water
Mud is mixed into combination ash with aluminium chloride；Water, fluid loss agent and antifoaming agent are put in the mixing container, blender is with low
(4000 ± 200 revs/min) of speed rotates, and the combination ash of above-mentioned oil-well cement and aluminium chloride is added in 15 seconds, covers and stirs
The lid of device is mixed, and continues stirring 35 seconds under high speed (12000 ± 500 revs/min), aluminium chloride cement mortar is made.
3, comparative example 2
It is prepared by " sodium metasilicate " cement mortar
Weigh 500g oil-well cements, 215g water, 0.5g antifoaming agent, 5g fluid loss agents, 7.5g sodium metasilicates.By oil-well cement
It is mixed into combination ash with sodium metasilicate；Water, fluid loss agent and antifoaming agent are put in the mixing container, blender is with low speed
(4000 ± 200 revs/min) rotate, and the combination ash of above-mentioned oil-well cement and sodium metasilicate is added in 15 seconds, cover blender
Lid, and continue stirring 35 seconds under high speed (12000 ± 500 revs/min), sodium metasilicate cement mortar be made.
4, prepared by the cement mortar containing free hydraulic control preparation
Weigh 500g oil-well cements, 215g water, 0.5g antifoaming agent, 5g fluid loss agents, free liquid prepared by 10g embodiments 1
Controlling agent.Water, fluid loss agent, antifoaming agent and free hydraulic control preparation are put in the mixing container, blender with low speed (4000 ±
200 revs/min) rotation, and the cement weighed is added in 15 seconds, the lid of blender is covered, and in high speed (12000 ± 500
Rev/min) under continue stirring 35 seconds, be made the 1 free hydraulic control preparation containing embodiment free liquid test cement mortar.
The above experiment is repeated five times, only free hydraulic control preparation changes the free hydraulic control of the preparation of embodiment 2,3,4,5,6 into respectively
Preparation, dosage are respectively 5g, 20g, 25g, 15g, 15g, obtain respectively containing embodiment 2, five parts of 3,4,5,6 free hydraulic control preparations
Free liquid tests cement mortar.
5, cement slurry property is tested
Following test methods are respectively adopted in every part of cement mortar of above-mentioned preparation：
It is conserved 20 minutes at 93 DEG C, six has been surveyed with six fast rotational viscometers (the sensible special instrument factory in Qingdao sea, ZNN-D6)
After speed value, pour into 250mL glass cylinders to 250mL graduation marks.The length of graduated cylinder 0~250mL scale parts is not lower than
232mm also should not be greater than 250mm, and 2mL or less is should be per lattice scale.During pouring into cement mortar, it is ensured that cement mortar sample
Product are uniform.Graduated cylinder tilts 45 °, and the time of repose of experiment is 2 hours, pours into graduated cylinder from cement mortar and counts.It will using plastic film
Graduated cylinder seals, to prevent moisture evaporation.After the time of repose for reaching 2 hours, the free liquid (cement in graduated cylinder of cement mortar is measured
Starch the transparent or colored liquid at top), it measures free fluid product and is at least accurate to ± 0.2mL.Test result, such as the following table 1.
The cement mortar rheological data of different embodiment controlling agent samples and free liquid test result is added in table 1
In terms of test result, add the cement mortar of 2.5g aluminium chlorides, cement mortar obtained very thickAdd cement mortar will be made further to thicken again, cannot pump, lose practical application
It may；And free liquid at this time is 1.3mL, there are no be effectively controlled.The cement mortar of up to 7.5g sodium metasilicates is added, from
It is 1.8mL by liquid, also without effectively controlling free liquid.The result shows that aluminium chloride cement mortar and sodium metasilicate cement mortar are simultaneously
It is not fully solved the control problem of free liquid in well cementation, still has free liquid, it cannot be separately as the freedom for stablizing maturation
Hydraulic control preparation.
Comparison shows that each embodiment rheological data height that free hydraulic control preparation is added turnsAll 300 hereinafter, simultaneously
Low turnWithIt is not high, it disclosure satisfy that cementing operation to cement paste rheological requirement.And each of free hydraulic control preparation is added
Embodiment, free liquid test is zero, illustrates that the free hydraulic control preparation of the present invention can effectively control the free liquid of cement mortar, is suitble to
The preparation of zero free liquid cement mortar.
Claims (10)
1. a kind of free hydraulic control preparation of cementing slurry, for include blending following components suspension：The green slope thread of nanometer
Stone, nano silicon dioxide, dispersant, slurry stabilizer and water；
Wherein, in terms of parts by weight, the parts by weight of water are 100 parts；
The nanometer attapulgite, 5~200nm of grain size, dosage are 10~30 parts；The nano silicon dioxide, grain size 10~
260nm, dosage are 20~40 parts；The dosage of the dispersant is 0.1~1 part, is disperseed selected from polycarboxylate dispersant, silane copolymer
At least one of agent or polysulfonate acid dispersant；The dosage of the slurry stabilizer be 0.5~1 part, selected from hydroxyethyl cellulose,
At least one of sodium carboxymethylcellulose, xanthans, scleroglucan, welan gum.
2. the free hydraulic control preparation of cementing slurry according to claim 1, it is characterised in that：
The polycarboxylate dispersant is selected from polyacrylic acid, maleic acid-acrylic acid copolymer, the copolymerization of acrylic acid-acrylic acid hydroxypropyl acrylate
Object, acrylic acid-acrylic ester-phosphonic acids-co-polymer of sulfonate, acrylic acid-acrylic ester-co-polymer of sulfonate, styrene-Malaysia
At least one of acid anhydride copolymer；
The silane copolymer dispersant is selected from polyether-modified Dimethicone Copolyol body, end group carries hydrolyzable silane
Key-Si (- O-CH3)3At least one of polymer；
The polysulfonate acid dispersant is selected from acrylic acid -2- acrylamide-2-methyl propane sulfonics copolymer, sodium pyrosulfite-formaldehyde -
At least one of acetone copolymer.
3. the free hydraulic control preparation of cementing slurry according to claim 2, it is characterised in that：
The polycarboxylate dispersant is selected from polyacrylic acid；The silane copolymer dispersant is selected from polyether-modified dimethyl silicone polymer
Copolymer；The polysulfonate acid dispersant is selected from sodium pyrosulfite-formaldehyde-acetone copolymer.
4. the free hydraulic control preparation of cementing slurry according to claim 1, it is characterised in that：
The nanometer attapulgite dosage is 20~30 parts；The nano silicon dioxide dosage is 20~30 parts.
5. the free hydraulic control preparation of cementing slurry according to claim 1, it is characterised in that：
The dispersant is 0.5~0.7 part；The slurry stabilizer is 0.5~0.6 part.
6. the free hydraulic control preparation of cementing slurry according to one of Claims 1 to 5, it is characterised in that：
The pH value of the suspension is 9~11.
7. the preparation method of the free hydraulic control preparation of cementing slurry according to one of claim 1~6 item includes that will wrap
It is uniformly mixed as suspension containing the component including the component.
8. the preparation method of the free hydraulic control preparation of cementing slurry according to claim 7, it is characterised in that：
After mixing by the component, adjust pH value to 9~11.
9. application of the cementing slurry with free hydraulic control preparation in cement mortar according to one of claim 1~6.
10. application of the cementing slurry according to claim 9 with free hydraulic control preparation in cement mortar, feature exist
In：
Cementing slurry is the 1~5% of cement weight with the addition of free hydraulic control preparation in the cement mortar.
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| CN107057665B (en) * | 2017-01-06 | 2019-10-25 | 中国海洋石油集团有限公司 | A kind of oleaginous suspension and its purposes for cementing slurry suspending agent |
| CN109265695B (en) * | 2018-08-24 | 2020-08-04 | 江南大学 | Preparation method and application of thickening modified xanthan gum |
| MY197237A (en) * | 2019-02-01 | 2023-06-07 | Halliburton Energy Services Inc | Compatible low crystalline silica spacers |
| CN111406754B (en) * | 2020-04-28 | 2021-06-15 | 浙江禾本科技股份有限公司 | Hexythiazox water suspending agent and preparation method thereof |
| CN113913167B (en) * | 2020-07-08 | 2023-05-30 | 中国石油化工股份有限公司 | Free liquid control agent for well cementation cement paste and preparation method and application thereof |
| CN114058346B (en) * | 2020-07-31 | 2023-03-14 | 中国石油化工股份有限公司 | Calcium silicate hydrate suspension and preparation method and application thereof |
| CN113105150A (en) * | 2021-02-23 | 2021-07-13 | 广东至道先进土木工程材料技术研究有限公司 | Suspension stabilizer, preparation method, use method and use device thereof |
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