CN109912792B - A kind of hardened oilwell cement water-swellable self-repair material and preparation method thereof - Google Patents
A kind of hardened oilwell cement water-swellable self-repair material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of hardened oilwell cement water-swellable self-repair material and preparation method thereof, belongs to oil drilling cementing technology field.The hardened oilwell cement water-swellable self-repair material is prepared by polyethylene glycol 400, DL- tartaric acid and the concentrated sulfuric acid, its weight ratio is 100:20~40:9~15, by preparing initial system solution, preparing water-swellable self-repair material solution, prepare three step of water-swellable self-repair material and be prepared.Water-swellable self-repair material rheological characteristic synthesized by the present invention is good, is convenient for conveying, and have no effect on the mechanical property of cement, when Behavior of Hardened Cement Paste generates microcrack and has water enchroachment (invasion) fashionable, it can respond rapidly to and generate complexation-crystallization object and repair microcrack, and Behavior of Hardened Cement Paste can be repaired repeatedly, it is extremely important to the durability and extension oil well service life that improve well-cementing cement.
Description
Technical field
The invention belongs to oil drilling cementing technology field, in particular to a kind of hardened oilwell cement water-swellable selfreparing material
Material and preparation method thereof.
Background technique
The main function of well-cementing cement is to realize oil, water Inter-zonal packing, prevents crossflow, guarantees that oil gas is raw safely
It produces.In order to realize this function, Behavior of Hardened Cement Paste must be continuous and impermeable.Due to the self-defect of cement material --- volume contraction
And brittleness, at present all there is Behavior of Hardened Cement Paste packing Problem of Failure i.e. Behavior of Hardened Cement Paste and crack occur in many oil/gas wells.Crack can reduce cement
The intensity of stone aggravates the chemical erosion of Behavior of Hardened Cement Paste, the serious durability for reducing Behavior of Hardened Cement Paste.
For the durability for improving hardened oilwell cement, hardened oilwell cement self-repair technology is got more and more attention.Existing oil well water
Mudstone, which meets water self-repair technology, mainly to be had: microcapsules of the admixture containing self-repair function in cement slurry, after microcapsules rupture certainly
Renovation agent fracture selfreparing；Patent CN108212036A discloses the formula and preparation process of a kind of self-repairing microcapsule.It should
The formula of the microcapsules with self-healing function of disclosure of the invention are as follows: using urea and formaldehyde as wall material, diglycidyl ether type epoxy
Resin is core material, but microcapsule method has that Strength Changes are larger, is easily broken during mixing slurry, and crack is being generated
When, the problem of microcapsules are difficult to rupture, and renovation agent cannot flow out.Addition has the water-absorbing resin of repair function in cement slurry,
At crack crack can be blocked with water swelling.It is disclosed in patent WO/2004/101952 and water swelling is added in cement slurry
Polymer, when crack, water flooding intrusion occurs in Behavior of Hardened Cement Paste, polymer absorption expands the method for blocking cement sheath crack.Specially
Sharp CN103044618A discloses a kind of preparation method of alkaline-resisting water-absorbing resin suitable for oil well cement paste.The water-absorbing resin with
Polyacrylamide, bentonite N,N-DMAA are monomer, carry out ternary polymerization and obtain water-absorbing resin.But these from
In recovery technique, water-absorbing resin, which exists, easily to absorb water, and be easy to cause cement slurry poor fluidity, is not easy the problem of pumping, to fail
It is practical at the scene.
Summary of the invention
The purpose of the present invention is to provide a kind of hardened oilwell cement water-swellable self-repair materials and preparation method thereof.The chance
When water expansion self-repair material makes an addition to cement slurry, cement slurry has good rheological property；It is formed when the grout cures
When Behavior of Hardened Cement Paste generates microcrack, which can respond rapidly to and repair microcrack；The preparation method uses
Raw material it is simple and easy to get, cheap, synthesis process is simple.
To reach the above technical purpose, the present invention the following technical schemes are provided:
A kind of hardened oilwell cement water-swellable self-repair material uses following Material synthesis with weight ratio meter:
100 parts of polyethylene glycol 400
20-40 parts of DL- tartaric acid
9~15 parts of the concentrated sulfuric acid
The molecular structural formula of the water-swellable self-repair material effective component are as follows:
Wherein, n=8~9, molecular weight are 874.09~950.09.
A kind of preparation method of hardened oilwell cement water-swellable self-repair material, comprising the following steps:
S1, it prepares initial system solution: taking the polyethylene glycol 400 of 100 parts by weight and the DL- tartaric acid of 20~40 parts by weight
It being added in clean container, sets 70~90 DEG C of reaction temperature, warming while stirring adds the concentrated sulfuric acid of 9~15 parts by weight,
With the increase in reaction time, DL- tartaric acid starts to dissolve, and apparent variation, isothermal reaction takes place in system solution viscosity
After a period of time, keep solution cooling in 20~25 DEG C of environment, gained is initial system solution, and entire reaction process continues
Stirring；
S2, it prepares water-swellable self-repair material solution: adjusting initial system solution obtained by S1 using pH adjusting agent
PH value is stood to 6.5~7.0, it is to be precipitated completely after separate to obtain supernatant and precipitating, by supernatant rotary evaporation to system solution
Until when viscosity is not further added by, volume no longer reduces；Precipitating is washed for several times and filtered with methanol solution, the rotation of gained filtrate is steamed
Until being sent to when system solution viscosity is not further added by, volume no longer reduces；Acquired solution after rotary evaporation twice is collected and merges,
As water-swellable self-repair material solution；
S3, it prepares water-swellable self-repair material: gained water-swellable self-repair material solution in step S2 is placed in 50
Dry 72~96h in~60 DEG C of vacuum oven obtains water-swellable self-repair material, also contains in resulting materials a certain amount of
Sulfate has certain auxiliaring effect to the repair process of water-swellable self-repair material.
Further, the mass fraction of the concentrated sulfuric acid is 75~98% in the step S2, the isothermal reaction time 2.5~
3.0h。
Further, pH adjusting agent is sodium carbonate liquor in the step S2.
Further, in the step S2, the rotary evaporation condition of supernatant are as follows: vacuum degree be 0.08~0.085MPa,
Temperature is 80~85 DEG C, revolving speed is 90~110r/min；The methanol cleaning solution rotary evaporation condition of precipitating are as follows: vacuum degree 0.08
~0.085MPa, temperature are 20~25 DEG C, revolving speed is 90~110r/min.
The invention has the benefit that
1, the cementing slurry containing water-swellable self-repair material synthesized by the present invention has good rheological property,
Guarantee that there is good pumpability when site operation.
2, prepared water-swellable self-repair material can be homogeneously dispersed in mortar architecture, and not influence cement
The original mechanical property of stone.
3, when there is water to penetrate into microcrack, water-swellable self-repair material of the invention can respond rapidly to and generate complexing
Crystal repairs microcrack, guarantees the continuous production of oil well, reduces because of well workover bring economic loss.
4, the well-cementing cement containing water-swellable self-repair material synthesized by the present invention can repair repeatedly microcrack, protect
The integrality for having demonstrate,proved Behavior of Hardened Cement Paste enhances the durability and stability of hardened oilwell cement, extends the Production Life of oil well.
Detailed description of the invention:
Fig. 1 is normal portland cement (control group) fracture end-face for being not added with water-swellable self-repair material of the present invention
Electron-microscope scanning figure, wherein a is its incipient crack end view drawing；B is that it conserves the fracture end-face after 28d in 80 DEG C, 20MPa water-bath
Figure.
Fig. 2 is the electron-microscope scanning for adding the normal portland cement fracture end-face of water-swellable self-repair material of the present invention
Figure, wherein c is its incipient crack end view drawing；D is that it conserves the fracture end-face figure after 28d in 80 DEG C, 20MPa water-bath.
Specific embodiment
The present invention is further described for 1-2 and embodiment with reference to the accompanying drawing.
Embodiment 1
100 parts of polyethylene glycol 400s and 20 parts of DL- tartaric acid are added in there-necked flask, set 70 DEG C of reaction temperature, side stirring
Side heating adds the concentrated sulfuric acid that 9 parts of mass fractions are 98%.With the increase in reaction time, DL- tartaric acid starts to dissolve,
System solution viscosity takes place apparent variation, after isothermal reaction 2.5h, keeps solution cooling in 25 DEG C of environment, gained is
For initial system solution；
The pH value for adjusting previous step obtained solution using sodium carbonate liquor stands, separates after precipitating completely to 6.5
Clear liquid and precipitating；Gained supernatant rotates steaming under conditions of vacuum degree is 0.08MPa, temperature is 80 DEG C, revolving speed is 95r/min
It is sent to stopping when solution viscosity is not further added by, volume no longer reduces；Precipitating is washed and is filtered, gained with a small amount of methanol solution 3 times
Filtrate under conditions of vacuum degree is 0.08MPa, temperature is 20 DEG C, revolving speed is 97r/min rotary evaporation to solution viscosity no longer
Increase, volume stop when no longer reducing；Collect and merge acquired solution after rotary evaporation twice, as water-swellable selfreparing material
Expect solution；
Water-swellable self-repair material solution is placed in dry 72h in the vacuum oven that temperature is 55 DEG C, it is swollen water must to be met
Swollen self-repair material (being denoted as 1#).
Embodiment 2
100 parts of polyethylene glycol 400s and 22 parts of DL- tartaric acid are added in there-necked flask, set 75 DEG C of reaction temperature, side stirring
Side heating adds the concentrated sulfuric acid that 10 parts of mass fractions are 98%.With the increase in reaction time, DL- tartaric acid starts to dissolve,
System solution viscosity takes place apparent variation, after isothermal reaction 2.5h, keeps solution cooling in 25 DEG C of environment, gained is
For initial system solution；
The pH value for adjusting initial system solution using sodium carbonate liquor is stood to 6.7, it is to be precipitated completely after separate to obtain supernatant
Liquid and precipitating；Gained supernatant rotates steaming under conditions of vacuum degree is 0.081MPa, temperature is 85 DEG C, revolving speed is 100r/min
It is sent to stopping when solution viscosity is not further added by, volume no longer reduces；Precipitating is washed 3 times with a small amount of methanol solution and is filtered, gained
Filtrate rotary evaporation under conditions of vacuum degree is 0.082MPa, temperature is 23 DEG C, revolving speed is 110r/min is glutinous to system solution
Stopping when degree is not further added by, volume no longer reduces；Collect acquired solution, as water-swellable selfreparing material after rotary evaporation twice
Expect solution；
Gained water-swellable self-repair material solution is placed in dry 84h in the vacuum oven that temperature is 55 DEG C, must be met
Water expands self-repair material (being denoted as 2#).
Embodiment 3
100 parts of polyethylene glycol 400s and 26 parts of DL- tartaric acid are added in there-necked flask, set 80 DEG C of reaction temperature, side stirring
Side heating adds the concentrated sulfuric acid that 10 parts of mass fractions are 98%.With the increase in reaction time, DL- tartaric acid starts to dissolve,
System solution viscosity takes place apparent variation, after isothermal reaction 3h, keeps solution cooling in 25 DEG C of environment, gained is
Initial system solution；
The pH value for adjusting initial system solution using sodium hydroxide solution is stood to 7.0, it is to be precipitated completely after separate
Clear liquid and precipitating；It is 0.083MPa that supernatant, which is placed in vacuum degree, and temperature is 84 DEG C, and revolving speed is revolved under the conditions of being 110r/min
Turn evaporation, until stopping when system solution viscosity is not further added by, volume no longer reduces；Precipitating is washed 3 times with a small amount of methanol solution
And filter, gained filtrate is 0.081MPa in vacuum degree, and temperature is 25 DEG C, and revolving speed carries out rotation steaming under the conditions of being 110r/min
Hair, until stopping when system solution viscosity is not further added by, volume no longer reduces；Acquired solution after rotary evaporation twice is collected, i.e.,
For water-swellable self-repair material solution；
Gained water-swellable self-repair material solution is placed in dry 72h in the vacuum oven that temperature is 55 DEG C, must be met
Water expands self-repair material (being denoted as 3#).
Embodiment 4
100 parts of polyethylene glycol 400s are added in there-necked flask and 30 parts of DL- tartaric acid (TA), warming while stirring add
The concentrated sulfuric acid that 12 parts of mass fractions are 98%；85 DEG C of reaction temperature of setting.With the increase in reaction time, DL- tartaric acid starts
Dissolution, system solution viscosity take place apparent variation, after isothermal reaction 3h, keep solution cooling in 25 DEG C of environment, institute
It must be initial system solution；
The pH value for adjusting initial system solution using sodium hydroxide solution is stood to 7.0, it is to be precipitated completely after separate
Clear liquid and precipitating；It is 0.085MPa that supernatant, which is placed in vacuum degree, and temperature is 85 DEG C, and revolving speed is revolved under the conditions of being 110r/min
Turn evaporation, until stopping when system solution viscosity is not further added by, volume no longer reduces；Precipitating is washed 3 times with a small amount of methanol solution
And filter, gained filtrate is 0.084MPa in vacuum degree, and temperature is 25 DEG C, and revolving speed carries out rotation steaming under the conditions of being 100r/min
Hair, until stopping when system solution viscosity is not further added by, volume no longer reduces；Acquired solution after rotary evaporation twice is collected, i.e.,
For water-swellable self-repair material solution；
Gained water-swellable self-repair material solution is placed in dry 96h in the vacuum oven that temperature is 55 DEG C, must be met
Water expands self-repair material (being denoted as 4#).
Performance test:
Selfreparing mortar architecture is prepared according to formula described in Tables 1 and 2, it is 25mm, height that cement slurry, which is poured into diameter,
For the cylindrical die of 50mm, maintenance 1d retreats mould in 80 DEG C, the water-bath of 20MPa, continues in 80 DEG C, the water-bath of 20MPa
Maintenance, respectively takes Behavior of Hardened Cement Paste 3 of example 1, example 2, example 3, example 4 and 2 control groups, passes through rock core displacement flow device
Permeability of (test condition are as follows: displacement pressure: 0.5MPa, confining pressure: the 2.5MPa) test in maintenance 0d, 7d, 14d, 28d.It is seeped
Saturating rate test result is listed in table 3 and table 4.
1 cement-slurry method 1 of table
Note: " SYJZ-1 " is dispersing agent, and " SWJ-1 " is fluid loss agent.Both the above additive is provided by Shengli Oil Field.
2 cement-slurry method 2 of table
| Sample | Good China's G class g cement/wt% | 3#/wt% | 4#/wt% | SYJZ-1/wt% | SWJ-1/wt% | Water/wt% |
| Example 3 | 100 | 5 | 0 | 0.3 | 1.5 | 44 |
| Example 4 | 100 | 0 | 5 | 0.3 | 1.5 | 44 |
| Control group | 100 | 0 | 0 | 0.3 | 1.5 | 44 |
Note: " SYJZ-1 " is dispersing agent, and " SWJ-1 " is fluid loss agent.Both the above additive is provided by Shengli Oil Field.
3 embodiment 1,2 of table and permeability variation in the selfreparing Behavior of Hardened Cement Paste maintenance processes of control group preparation
4 embodiment 3,4 of table and permeability variation in the selfreparing Behavior of Hardened Cement Paste maintenance processes of control group preparation
The experimental result as shown in above-mentioned table 3, table 4 is it is found that be added to repairing for the Behavior of Hardened Cement Paste of water-swellable self-repair material
Reactivation power is substantially better than the Behavior of Hardened Cement Paste for being not added with water-swellable self-repair material: the cement added with water-swellable self-repair material
Stone can microcrack generate respond rapidly within first 7 days and can preceding 14 angel have microcrack Behavior of Hardened Cement Paste permeability drop
Down within 0.1mD, show that added water-swellable self-repair material has good repairing performance；In the maintenance week of 28d
After phase, the Behavior of Hardened Cement Paste permeability of four experimental groups is respectively less than 0.1mD, and far smaller than two groups of control Behavior of Hardened Cement Paste are in 30-45mD
Between permeability；And the Behavior of Hardened Cement Paste that water-swellable self-repair material is added to it can be seen from attached drawing can be to Behavior of Hardened Cement Paste
Microcrack is automatically repaired, and ensure that the integrality of Behavior of Hardened Cement Paste.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, but anything that does not depart from the technical scheme of the invention content, according to the technical essence of the invention
Any simple modification, equivalent change and modification to the above embodiments, all of which are still within the scope of the technical scheme of the invention.
Claims (5)
1. a kind of hardened oilwell cement water-swellable self-repair material, which is characterized in that with weight ratio meter, the water-swellable is reviewed one's lessons by oneself
The multiple following Material synthesis of materials'use:
100 parts of polyethylene glycol 400
20-40 parts of DL- tartaric acid
9~15 parts of the concentrated sulfuric acid
The effective component molecular structural formula of the water-swellable self-repair material are as follows:
Wherein, n=8~9, molecular weight are 874.09~950.09.
2. a kind of preparation method of hardened oilwell cement water-swellable self-repair material as described in claim 1, including following step
It is rapid:
S1, prepare initial system solution: the DL- tartaric acid of the polyethylene glycol 400,20~40 parts by weight that take 100 parts by weight is added
In clean container, 70~90 DEG C of reaction temperature are set, adds the concentrated sulfuric acid of 9~15 parts by weight, isothermal reaction is entire to react
Process persistently stirs, and after reaction, keeps solution cooling in 20~25 DEG C of environment, gained is initial system solution；
S2, it prepares water-swellable self-repair material solution: adjusting the pH value of initial system solution obtained by S1 using pH adjusting agent
To 6.5~7.0, stand, it is to be precipitated completely after separate to obtain supernatant and precipitating, supernatant rotary evaporation to its viscosity is no longer increased
Add, when volume no longer reduces until；Precipitating is washed for several times and filtered with methanol solution, gained filtrate rotary evaporation to its viscosity
Be not further added by, when volume no longer reduces until；It collects and merges acquired solution after rotary evaporation twice, as water-swellable is reviewed one's lessons by oneself
Multiple material solution；
S3, water-swellable self-repair material is prepared, gained water-swellable self-repair material solution in step S2 is placed in 50~60
DEG C vacuum oven in after dry 72~96h to get water-swellable self-repair material.
3. a kind of preparation method of hardened oilwell cement water-swellable self-repair material according to claim 2, feature exist
In the mass fraction of the concentrated sulfuric acid is 75~98% in the step S1,2.5~3.0h of isothermal reaction time.
4. a kind of preparation method of hardened oilwell cement water-swellable self-repair material according to claim 2, feature exist
In the pH adjusting agent is sodium carbonate liquor.
5. a kind of preparation method of hardened oilwell cement water-swellable self-repair material according to claim 2, feature exist
In, in the step S2, the rotary evaporation condition of supernatant are as follows: vacuum degree is 0.08~0.085MPa, temperature is 80~85 DEG C,
Revolving speed is 90~110r/min；The methanol cleaning solution rotary evaporation condition of precipitating are as follows: vacuum degree is 0.08~0.085MPa, temperature
It is 90~110r/min for 20~25 DEG C, revolving speed.
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| CN113698612A (en) * | 2021-09-27 | 2021-11-26 | 中国石油化工股份有限公司 | Microcapsule for cement stone self-repairing and preparation method thereof |
| CN114149191B (en) * | 2022-02-09 | 2022-05-03 | 胜利油田渤海固井工程技术有限责任公司 | Water-swelling agent for oil well cement and preparation method thereof |
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| CN105693946A (en) * | 2016-01-25 | 2016-06-22 | 湖南省建筑工程集团总公司 | Anti-crack high slump loss resistance concrete polycarboxylate superplasticizer |
| CN106892594B (en) * | 2017-02-20 | 2020-07-10 | 中国石油化工股份有限公司 | Micro-expansion toughened cement slurry and preparation method thereof |
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