CN104418965A - Preparation method of self-healing agent for oil well cement, well cementation self-healing cement slurry and application - Google Patents
Preparation method of self-healing agent for oil well cement, well cementation self-healing cement slurry and application Download PDFInfo
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Abstract
The invention discloses a preparation method of a self-healing agent for oil well cement. The preparation method comprises the following steps: i) mixing substituted or unsubstituted styrene, acrylates, 2-acrylamide-2-methyl propane sulfonic acid, divinyl benzene, acrylamide and derivatives thereof, mono polyethylene glycol maleate, an emulsifier and a chain transfer agent with water and pre-emulsifying to obtain a pre-emulsion A; ii) preparing an initiator solution B by water and an initiator; iii) heating a part amount of the pre-emulsion A to 70-90 DEG C and then adding a part amount of the initiator solution B; then, further adding the residual amount of the pre-emulsion A and the initiator solution B; and iv) after reaction, adjusting the pH value to 7-9 to obtain the self-healing agent for oil well cement. The invention further relates to well cementation self-healing cement slurry which contains the self-healing agent prepared by the method as well as an application of the self-healing agent or the well cementation self-healing cement slurry in oil gas well cementing operation.
Description
Technical field
The present invention relates to petroleum exploration field, be specifically related to the oil well self-healing grout that the self-healing mixture that the method prepares is prepared and contained to a kind of oil well cement self-healing mixture, more specifically, it relates to a kind of preparation method and and the well cementation self-healing grout of self-healing mixture for preparing containing the method and application thereof of a kind of oil well cement self-healing mixture of deep well cementing.
Background technology
Oil/gas Well is after cement slurry sets, due to the impact of cement self-characteristic or later stage operation, easily the defects such as crack are formed in Behavior of Hardened Cement Paste, because cement mantle damage occurs that oil gas channelling causes annular space situation with pressure to occur, later stage generally adopts the large well workover of the squeeze method of cost intensive and chemical plugging restorative procedure, but success ratio is low, some repairs need to carry out many times, and the Oil/gas Well after repairing often may go wrong again in a short period of time, need again to repair, often cause the prolongation in a large amount of financial losses and drilling operation cycle, at present, domestic and international each large oil play, scientific research institutions are also being devoted to solve Behavior of Hardened Cement Paste damage, the research of selfreparing, but there is no the disclosed preparation about self-healing mixture.The selfreparing research starting comparatively morning of domestic construction industry cement-based material microfracture, but the self-healing mixture of building trade is lower due to use temperature, is difficult to be applied in oil well cement.Abroad have made some progress in the research and use of the selfreparing of cementing concrete ring, Schlumberger and Halliburton are in the research in cement mantle damage, cement mantle microdilatancy, but the renovation agent had research and development are not yet open.
Benzene emulsion disclosed in Chinese patent patent CN201010531412.X, CN201210587842.2, CN201110375710.9, CN201010530012.7 etc. is only applicable to building trade, coating industry etc., be difficult to be suitable in the High Temperature High Pressure oil well of temperature higher than 100 DEG C, and add in oil well cement, cause oil well cement without mobility, be difficult to be pumped into well.
The self-healing mixture that Chinese patent CN201010617895.5, CN201310031979.4 invent is only applicable to the construction cement under normal temperature, cannot work for the oil well cement under high temperature.
Chinese patent CN201110326575.9 utilizes modified resin as self-healing material, but the use temperature of this material is at about 70 DEG C; Chinese patent CN201210264282.7 does not provide the preparation method of self-healing material.
Summary of the invention
The object of the present invention is to provide a kind of method preparing oil well cement self-healing mixture, self-healing mixture prepared by the method can at high temperature repair Behavior of Hardened Cement Paste crack, reduce Behavior of Hardened Cement Paste rate of permeation, packing oil gas water channeling passage, prevent the generation of channelling, improve bonding quality and the weather resistance of cementing concrete ring, ensure good packing, improve work-ing life and the development benefit of Oil/gas Well.
To achieve these goals, the invention provides following technical scheme:
1) preparation method for oil well cement self-healing mixture, comprising:
I) by substituted or unsubstituted, pre-emulsification is carried out in vinylbenzene, esters of acrylic acid, 2-acrylamide-2-methyl propane sulfonic, Vinylstyrene, acrylamide and the mixing of derivative, mono polyethylene glycol maleate, emulsifying agent, chain-transfer agent and water thereof, obtain pre-emulsion A;
Ii) water and initiator are made into initiator solution B;
Iii) the pre-emulsion A of part amount is heated to 70-90 DEG C as bed material, the initiator solution B then adding part amount reacts;
Iv) the pre-emulsion A of residual content and the initiator solution B of residual content is also added wherein react further subsequently;
V), after reaction terminates, the pH value regulating product is 7-9, obtains described oil well cement self-healing mixture.
Wherein preferred steps ii) in the usage quantity of water be 20 % by weight of the usage quantity of whole water.
2) the of the present invention 1st) in the preferred implementation of preparation method described in item, in described method, the add-on of each component is:
3) the of the present invention 1st) or the 2nd) in the preferred implementation of preparation method described in item, in described method, the add-on of each component is:
4) the of the present invention 1st)-3) according to any one of preparation method an embodiment in, described esters of acrylic acid is selected from least one in methyl acrylate, ethyl propenoate, butyl acrylate, octadecyl acrylate, methyl methacrylate and butyl methacrylate.
5) the of the present invention 1st)-4) according to any one of preparation method an embodiment in, described emulsifying agent is selected from anion surfactant and/or nonionogenic tenside; Described anion surfactant is selected from least one in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, alkyl phenol ether sulfo-succinic acid ester sodium salt and alkyl ether sulfate salt; Described nonionogenic tenside is selected from least one in Octylphenol polyoxyethylene ether, polyoxyethylene nonylphenol ether, ethoxylated dodecyl alcohol and glycol fatty acid ester.
6) the of the present invention 1st)-5) according to any one of preparation method an embodiment in, described initiator is selected from inorganic peroxide compounds, is preferably at least one in Potassium Persulphate, Sodium Persulfate and ammonium persulphate.
7) the of the present invention 1st)-6) according to any one of preparation method an embodiment in, described chain-transfer agent is alcohols, is preferably at least one in Virahol, lauryl mercaptan and the trimethyl carbinol.
8) a kind of well cementation self-healing grout, comprises the of the present invention 1st)-7) the oil well cement self-healing mixture prepared of preparation method described in item.
9) in the present invention the 8th) in an embodiment of well cementation self-healing grout described in item, described well cementation self-healing grout comprises:
Oil well cement 100 weight part; With
Described oil well cement self-healing mixture 5-20 weight part.
10) a kind of the present invention the 1st)-7) the oil well cement self-healing mixture or the 8th prepared of method according to any one of item) or the 9th) application of well cementation self-healing grout in oil gas well cementing operation described in item.
Added in cementing concrete by oil well cement self-healing mixture of the present invention and formed in described well cementation self-healing grout (also referred to as well cementation self-healing mortar architecture), it effectively can increase the compactness of oil well cement; Reduce the filter loss of grout; The chance oil realized under Behavior of Hardened Cement Paste hot conditions expands, and reduces the rate of permeation under Behavior of Hardened Cement Paste high temperature, and effective prevention effectively prevents the has channeling of well cementation section from occurring, and improves oil gas well cementing operation quality.
General is 100 weight parts with cement content in cementing slurry, oil well cement self-healing mixture of the present invention for 5-20 weight part is added cementing slurry, mixes.
Cementing slurry is some the cement paste for well cementation systems commonly used in prior art.The present invention plants preferably can contain following component:
Wherein, oil well cement is good magnificent G level oil well cement; Silica flour is conventional extra material in cementing system; Water retaining, dispersion agent and retardant can adopt admixture conventional in cementing system; Above extra material, admixture all can by commercially available and obtain.
After adopting such scheme, because the present invention takes following measures:
1. the present invention selects oil-soluble monomer vinylbenzene, esters of acrylic acid emulsion polymerization to synthesize oil suction swelling type self-healing mixture, and the tridimensional network molecule of this self-healing particle has very strong oil absorption.Therefore, self-healing particle of the present invention joins in grout, after cement slurry sclerosis, has certain chance oil expansion function.After cracking or generation annular space occur oil well cement sleeve pipe, Sweet natural gas or oil infiltrate crack, self-healing particle generation volumetric expansion, thus repair shutoff crack, reach the function improving cement mantle impermeability.
2. the 2-acrylamide-2-methyl propane sulfonic (AMPS) added in synthesis, it is a kind of vinyl monomer with sulfonic acid group, there is good thermostability, decomposition temperature reaches as high as 210 DEG C, therefore, the more conventional styrene-acrylic latex of the self-healing mixture gone out synthesized by the present invention has more good salt resistance, high thermal resistance; During the more conventional styrene-acrylic latex of self-healing mixture of the present invention is more suitable for can sending out for the Oil/gas Well of High Temperature High Pressure.In addition, the amide group contained in 2-acrylamide-2-methyl propane sulfonic (AMPS), makes self-healing mixture have good stability to hydrolysis, thermostability.
3. the Vinylstyrene introduced in synthesis has two ethyl alkene, can generate the self-healing mixture of three-dimensional structure when being polymerized.
4. mono polyethylene glycol maleate (MPEGMA) molecule is with hydrophilic carboxyl, carboxyl hydratability is stronger, can be interacted by electrostatic and cement granules and adsorb, therefore, the self-healing mixture gone out synthesized by the present invention makes oil well cement paste have excellent rheological property and degree of mobilization, is easy to on-the-spot construction pumping.
Therefore the present invention has the following advantages:
1) the self-healing mixture synthesized by the present invention is owing to having sulfonic acid group, amide group, benzene ring structure, and more conventional benzene emulsion more can bear high temperature, the high pressure of down-hole; Self-healing cement slurry ties up to 150 DEG C, still can reach the effect of meeting oil and expanding under 21MPa.
2) self-healing particle has tridimensional network, lipophilic group, effectively can reach the effect of meeting oil and expanding.
3) hydroxy-acid group in self-healing particle makes self-healing particle in oil well cement, serves dispersion and lubrication; The oil well cement paste being added with self-healing particle is easier to on-the-spot construction pumping.
4) self-healing particle is assembled under differential pressure, is formed with the latex film of some strength, prevents gas from invading in grout; Reduce the surface tension of grout, make to alter into minimum gas be dispersed into microvesicle, these microvesicles are in bond, can not gather and alter formation gas passage; After the static gel strength of grout is formed, self-healing is particle-filled in the space of cement granules, decreases the microfissure that hydrated cementitious causes, reduces rate of permeation, and the has channeling of the section that effectively prevents from cementing the well occurs, and improves oil gas well cementing operation quality.
In addition, invention also has following beneficial effect:
1. when cracking occurs oil well cement sleeve pipe or after producing annular space, Sweet natural gas or oil infiltrate crack, self-healing particle generation volumetric expansion of the present invention, thus repair shutoff crack, effectively reduce the rate of permeation of oil well cement, reach the function improving cement mantle impermeability.
The use temperature of the self-healing mixture 2. gone out synthesized by the present invention can reach 120 DEG C, and demulsifying phenomenon does not occur.
3. the self-healing mixture gone out synthesized by the present invention makes oil well cement paste have excellent rheological property and degree of mobilization, is easy to on-the-spot construction pumping.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail, but scope of the present invention is not limited to following examples.
The preparation method of oil well cement self-healing mixture of the present invention can be concrete comprise:
Specifically method of the present invention can also be:
I) pre-emulsification is carried out in vinylbenzene, esters of acrylic acid, 2-acrylamide-2-methyl propane sulfonic, Vinylstyrene, acrylamide and derivative thereof, mono polyethylene glycol maleate, emulsifying agent, chain-transfer agent and deionized water (80% of total Water) mixing, obtain pre-emulsion A;
Ii) deionized water of total Water 20% and initiator are made into initiator solution B to carry out;
Iii) using the pre-emulsion A of part amount as bed material, drop in reactor and be heated to 70-90 DEG C, the initiator solution B then adding part amount reacts;
Iv) by the pre-emulsion A of residual content and the initiator solution B of residual content, instill in reactor in 4-6h simultaneously, drip after terminating, continue reaction 1-2h;
V), after reaction terminates, the pH value regulating product is 7-9, obtains described oil well cement self-healing mixture.
The oil well cement preparation embodiment of self-healing mixture
Embodiment 1
Step 1) is by vinylbenzene 70 weight part, acrylate 40 weight part, 2-acrylamide-2-methyl propane sulfonic 15 weight part, Vinylstyrene 1 weight part, acrylamide 9 weight part, mono polyethylene glycol maleate 1 weight part, emulsifying agent 0.7 weight part, chain-transfer agent 0.1 weight part, deionized water 120 weight part (80% of total Water 150 weight part), pre-emulsification, obtains pre-emulsion A;
Step 2) deionized water 30 weight part (20% of total Water 150 weight part) and initiator 0.7 weight part are made into initiator solution B;
The pre-emulsion A of 20 % by weight adds in reactor as bed material by step 3), and heating, stirring, be warming up to 90 DEG C, and add in reactor by the initiator solution B of 20 % by weight;
Step 4), by the initiator solution B of the pre-emulsion A of residue 80 % by weight with residue 80% amount, instills in reactor in 5h simultaneously, drips after terminating, and continues reaction 1h;
After step 5) reaction terminates, be cooled to room temperature, adjust pH is 7-9.Namely oil well cement self-healing mixture 1 is obtained
#.
Embodiment 2
Step 1) is by vinylbenzene 50 weight part, acrylate 55 weight part, 2-acrylamide-2-methyl propane sulfonic 20 weight part, Vinylstyrene 5 weight part, acrylamide 7 weight part, mono polyethylene glycol maleate 7 weight part, emulsifying agent 2.5 weight part, chain-transfer agent 0.3 weight part, deionized water 280 weight part (80% of total Water 350 weight part), pre-emulsification, obtains pre-emulsion A;
Step 2) deionized water 70 weight part (20% of total Water 350 weight part) and initiator 2.5 weight part are made into initiator solution B;
The pre-emulsion A of 20 % by weight adds in reactor as bed material by step 3), and heating, stirring, be warming up to 70 DEG C, and add in reactor by the initiator solution B of 20 % by weight;
Step 4), by the initiator B of the pre-emulsion A of residue 80% amount with residue 80% amount, instills in reactor in 6h simultaneously, drips after terminating, and continues reaction 1h;
After step 5) reaction terminates, be cooled to room temperature, the pH value regulating product is 7-9.Namely oil well cement self-healing mixture 2 is obtained
#.
Embodiment 3
Step 1) is by vinylbenzene 60 weight part, acrylate 45 weight part, 2-acrylamide-2-methyl propane sulfonic 18 weight part, Vinylstyrene 3 weight part, acrylamide 7.5 weight part, mono polyethylene glycol maleate 6.5 weight part, emulsifying agent 2 weight part, chain-transfer agent 0.2 weight part, deionized water 240 weight part (80% of total Water 300 weight part), pre-emulsification, obtains pre-emulsion A;
Step 2) deionized water 60 weight part (20% of total Water 300 weight part) and initiator 2 weight part are made into initiator solution B;
The pre-emulsion A of 20 % by weight adds in reactor as bed material by step 3), and heating, stirring, be warming up to 90 DEG C, and add in reactor by the initiator solution B of 20 % by weight;
Step 4), by the initiator solution B of the pre-emulsion A of residue 80 % by weight with residue 80 % by weight amounts, instills in reactor in 6h simultaneously, drips after terminating, and continues reaction 1h;
After step 5) reaction terminates, be cooled to room temperature, the pH value regulating product is 7-9.Namely oil well cement self-healing mixture 3 is obtained
#.
Application Example:
Embodiment 4
Well cementation self-healing grout: good magnificent G level oil well cement is 100 parts of weight, the quartz sand of 35 parts, the fluid loss agent of 5 parts, the dispersion agent of 2 parts, the retardant of 3.5 parts, the self-healing mixture 1 of 5 parts
#, 2
#, 3
#.
The Behavior of Hardened Cement Paste of the self-healing mixture being added with the present embodiment being carried out man seam respectively, putting into making the Behavior of Hardened Cement Paste after seam the special high-temperature high-pressure curing still being added with diesel oil, 100 DEG C, maintenance after 1 day, 7 days, 14 days under 5MPa, the rate of permeation of test water mudstone.Test-results is in table 1.
Under 100 DEG C, table 1,5MPa, Behavior of Hardened Cement Paste repairs information slip
Embodiment 5
Well cementation self-healing grout: good magnificent G level oil well cement is 100 parts of weight, the quartz sand of 35 parts, the fluid loss agent of 5 parts, the dispersion agent of 2 parts, the retardant of 3.5 parts, the self-healing mixture 1 of 15 parts
#, 2
#, 3
#.
The Behavior of Hardened Cement Paste of the self-healing mixture being added with the present embodiment being carried out man seam respectively, putting into making the Behavior of Hardened Cement Paste after seam the special high-temperature high-pressure curing still being added with diesel oil, 110 DEG C, maintenance after 1 day, 7 days, 14 days under 5MPa, the rate of permeation of test water mudstone.Test-results is in table 2.
Under 110 DEG C, table 2,5MPa, Behavior of Hardened Cement Paste repairs information slip
Embodiment 6
Well cementation self-healing grout: good magnificent G level oil well cement is 100 parts of weight, the quartz sand of 35 parts, the fluid loss agent of 5 parts, the dispersion agent of 2 parts, the retardant of 3.5 parts, the self-healing mixture 1 of 20 parts
#, 2
#, 3
#.
The Behavior of Hardened Cement Paste of the self-healing mixture being added with the present embodiment being carried out man seam respectively, putting into making the Behavior of Hardened Cement Paste after seam the special high-temperature high-pressure curing still being added with diesel oil, 120 DEG C, maintenance after 1 day, 7 days, 14 days under 5MPa, the rate of permeation of test water mudstone.Test-results is in table 3.
Under 120 DEG C, table 3,5MPa, Behavior of Hardened Cement Paste repairs information slip
Can be found out by table 1, table 2, table 3, do not add the Behavior of Hardened Cement Paste of self-healing mixture, permeability resume figure does not have considerable change; Be added with the Behavior of Hardened Cement Paste of self-healing mixture of the present invention after 100 DEG C, 110 DEG C, 120 DEG C maintenances, permeability reduction, self-healing mixture is described at high temperature without decomposition, the self-healing mixture namely synthesized by the present invention is applicable to the down-hole of high temperature, high pressure; The self-healing dosage be added with in Behavior of Hardened Cement Paste is more, and the rate of permeation of maintenance Behavior of Hardened Cement Paste after 7 days, 14 days is lower.
Claims (10)
1. an oil well cement preparation method for self-healing mixture, comprising:
I) pre-emulsification is carried out in substituted or unsubstituted vinylbenzene, esters of acrylic acid, 2-acrylamide-2-methyl propane sulfonic, Vinylstyrene, acrylamide and the mixing of derivative, mono polyethylene glycol maleate, emulsifying agent, chain-transfer agent and water thereof, obtain pre-emulsion A;
Ii) water and initiator are made into initiator solution B;
Iii) the pre-emulsion A of part amount is heated to 70-90 DEG C as bed material, the initiator solution B then adding part amount reacts;
Iv) the pre-emulsion A of residual content and the initiator solution B of residual content is also added wherein react further subsequently;
V), after reaction terminates, the pH value regulating product is 7-9, obtains described oil well cement self-healing mixture.
2. method according to claim 1, is characterized in that, in described method, the add-on of each component is:
3. method according to claim 1 and 2, is characterized in that, in described method, the add-on of each component is:
4. the method according to any one of claim 1-3, is characterized in that, described esters of acrylic acid is selected from least one in methyl acrylate, ethyl propenoate, butyl acrylate, octadecyl acrylate, methyl methacrylate and butyl methacrylate.
5. the method according to any one of claim 1-4, is characterized in that, described emulsifying agent is selected from anion surfactant and/or nonionogenic tenside; Described anion surfactant is selected from least one in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, alkyl phenol ether sulfo-succinic acid ester sodium salt and alkyl ether sulfate salt; Described nonionogenic tenside is selected from least one in Octylphenol polyoxyethylene ether, polyoxyethylene nonylphenol ether, ethoxylated dodecyl alcohol and glycol fatty acid ester.
6. the method according to any one of claim 1-5, is characterized in that, described initiator is selected from inorganic peroxide compounds, is preferably at least one in Potassium Persulphate, Sodium Persulfate and ammonium persulphate.
7. the method according to any one of claim 1-6, is characterized in that, described chain-transfer agent is alcohols, is preferably at least one in Virahol, lauryl mercaptan and the trimethyl carbinol.
8. a well cementation self-healing grout, comprises oil well cement self-healing mixture prepared by the preparation method according to any one of claim 1-7.
9. well cementation self-healing grout according to claim 8, is characterized in that, described well cementation self-healing grout comprises:
Oil well cement 100 weight part; With
Described oil well cement self-healing mixture 5-20 weight part.
10. oil well cement self-healing mixture prepared by the method according to any one of a claim 1-7 or the application of well cementation self-healing grout in oil gas well cementing operation described in claim 8 or 9.
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| CN109251736A (en) * | 2018-10-16 | 2019-01-22 | 中国石油集团渤海钻探工程有限公司 | Self-healing cement slurry suitable for the well cementation of clastic rock well |
| CN113248169A (en) * | 2021-05-26 | 2021-08-13 | 天津大学 | Self-healing organic-inorganic composite cement-based self-healing agent based on self-healing, preparation method and application |
| CN113248169B (en) * | 2021-05-26 | 2022-09-20 | 天津大学 | Self-healing organic-inorganic composite cement-based self-healing agent based on self-healing, preparation method and application |
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