CN116063050A - Carbon dioxide corrosion resistant self-healing cement system - Google Patents
Carbon dioxide corrosion resistant self-healing cement system Download PDFInfo
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- CN116063050A CN116063050A CN202310207026.2A CN202310207026A CN116063050A CN 116063050 A CN116063050 A CN 116063050A CN 202310207026 A CN202310207026 A CN 202310207026A CN 116063050 A CN116063050 A CN 116063050A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/34—Non-shrinking or non-cracking materials
- C04B2111/343—Crack resistant materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
The invention discloses a carbon dioxide corrosion resistant self-repairing cement system, and relates to the technical field of special cement. The self-repairing cement system comprises Portland cement, and further comprises water-soluble linear diamine, an epoxy compound, nano silicon dioxide and hydroxyapatite, wherein the water-soluble linear diamine accounts for 1-2% of the Portland cement, the epoxy compound accounts for 0.3-1.5% of the Portland cement, the nano silicon dioxide accounts for 1-3% of the Portland cement, and the hydroxyapatite accounts for 1-2.5% of the Portland cement. The self-repairing cement system is applied to a high-pressure carbon dioxide environment, and can perform self-repairing under the environment, and has stronger repairing performance; and also can resist carbon dioxide corrosion, thus being applicable to some constructions with high-pressure carbon dioxide environments.
Description
Technical Field
The invention relates to the technical field of special cement, in particular to a carbon dioxide corrosion resistant self-repairing cement system.
Background
There are currently two main approaches to reduce "carbon emissions": firstly, the emission of carbon dioxide is reduced from the source, and secondly, the carbon dioxide in the atmosphere is fixed. Wherein, fixing carbon dioxide mainly comprises plant absorption, ocean sequestration and carbon dioxide capture. At present, most of the staff send the captured carbon dioxide into the underground for storage, and under the high pressure condition, the carbon dioxide is adsorbed by underground fluid or rock stratum, so that the carbon dioxide can be effectively stored.
However, for underground burying of carbon dioxide, after the carbon dioxide is buried underground, a cement stone structure is generally used for sealing the carbon dioxide so as to avoid the carbon dioxide overflowing the ground. However, in the long-term working of cement, certain cracks can be generated, so that leakage of carbon dioxide, strength reduction of cement stone and service life reduction are caused; meanwhile, carbon dioxide can corrode the cement stone, so that the strength of the cement stone is low, the permeability of the cement stone is high, and the service life of the cement stone is also reduced.
Disclosure of Invention
In view of the above technical problems, the present invention aims to overcome the defects of the prior art, and provide a carbon dioxide corrosion resistant self-repairing cement system, which can perform self-repairing under the condition of high-pressure carbon dioxide and has good carbon dioxide corrosion resistance.
The invention adopts the following technical scheme:
the self-repairing cement system resistant to carbon dioxide corrosion comprises Portland cement, and further comprises water-soluble linear diamine, an epoxy compound, nano silicon dioxide and hydroxyapatite, wherein the water-soluble linear diamine accounts for 1-2% of the Portland cement, the epoxy compound accounts for 0.3-1.5% of the Portland cement, the nano silicon dioxide accounts for 1-3% of the Portland cement, and the hydroxyapatite accounts for 1-2.5% of the Portland cement.
Among them, for the underground carbon dioxide storage, portland cement, including G-class oil well cement, etc., are generally used, and these are common cement varieties in the art. For the water-soluble linear diamine, the epoxy compound, the nano silicon dioxide and the hydroxyapatite, the water-soluble linear diamine, the epoxy compound, the nano silicon dioxide and the hydroxyapatite are added into cement paste before curing and forming the cement paste, so that the additives are uniformly mixed with silicate cement, and then the cement paste is cured and formed.
The water-soluble linear diamine and epoxy compound are added to cement because they react with carbon dioxide under high pressure: the water-soluble linear diamine and carbon dioxide form polyureas under high pressure conditions, and the epoxy compound and carbon dioxide form polycarbonates and small amounts of carbonates under high pressure conditions. Carbon dioxide gas enters the inside of the crack after the cement stone generates the crack, meanwhile, water-soluble linear diamine and epoxy compounds in the crack are exposed and react with carbon dioxide, and finally generated polyurea and polycarbonate can fill the crack, meanwhile, the integral strength of the cement stone cannot be reduced due to higher strength of the polyurea and the polycarbonate, and meanwhile, the carbonate has certain viscosity, so that the stability of the polyurea and the polycarbonate in filling the crack can be improved.
For nano silicon dioxide and hydroxyapatite, the combination of the nano silicon dioxide and the hydroxyapatite can effectively reduce the corrosion of carbon dioxide to cement stone. For CSH structure of cement stone, it belongs to a gel structure, contains a large number of nanometer scale pores inside, and the added nanometer silica can well fill the pores, so as to effectively improve the pore structure of cement stone; meanwhile, the added nano silicon dioxide can also play a role of crystal nucleus in the cement hydration process, so that crystallization and precipitation of hydration products are accelerated, hydration reaction is promoted to be carried out forward, the hydration speed of cement can be further improved, and the hole type performance and mechanical property of cement stone are improved; meanwhile, the specific surface area of the nano silicon dioxide is large, and the activity is relatively high, so that the alkalinity of the cement can be reduced, and the carbon dioxide corrosion resistance of the cement is improved. And for the hydroxyapatite, the concentration of calcium hydroxide on the surface of the cement stone can be effectively reduced, and the permeability of the cement stone can be reduced, so that the carbon dioxide corrosion resistance of the cement stone can be well improved.
After the four substances are mixed with cement and hardened and formed, the nano silicon dioxide and the hydroxyapatite can well increase the carbon dioxide corrosion resistance of the cement before the cement is cracked. When the cement stone generates cracks, the pressure of the carbon dioxide in the ground gas storage can reach several megapascals or even tens of megapascals, so that the water-soluble linear diamine and the epoxy compound can react with the carbon dioxide to repair the cracks, and the cement stone is self-repaired due to the fact that small granular substances exist in the cement stone; meanwhile, at the moment, the nano silicon dioxide and the hydroxyapatite can still play the roles of the nano silicon dioxide and the hydroxyapatite, so that the overall corrosion resistance of the cement stone is improved, and the strength of the cement stone is prevented from being reduced under the action of carbon dioxide.
Meanwhile, the inventor finds that when the addition of each material is controlled according to the following proportion, the self-repairing cement system formed finally has better performance: the water-soluble linear diamine accounts for 1.4-1.6% of the Portland cement, the epoxy compound accounts for 0.8-1.0% of the Portland cement, the nano silicon dioxide accounts for 1.8-2.2% of the Portland cement, and the hydroxyapatite accounts for 1.6-2.0% of the Portland cement
One embodiment of the invention is that the water-soluble linear diamine is one of ethylenediamine, 1, 4-butanediamine, 1, 5-pentanediamine and hexamethylenediamine; the epoxy compound is butylene oxide. The linear diamine is required to have water solubility because it is more easily mixed with cement uniformly, and the chain length of the water-soluble linear diamine is not easily too long, and the longer the chain length is, the lower the reaction rate and efficiency are, resulting in poor repairing effect, so that one of ethylenediamine, 1, 4-butanediamine, 1, 5-pentanediamine, and hexanediamine is preferable. More preferably, 1, 4-butanediamine is selected to have better effect. In the case of epoxy compounds, all epoxy compounds can be theoretically used in the invention, but in terms of practical effect, the boiling points of ethylene oxide and propylene oxide are too low, so that the epoxy compounds are easy to volatilize, and a large number of air holes are generated in the cement stone when the epoxy compounds volatilize in the process of cement solidification molding, so that the strength of the cement stone is low; while the higher molecular weight of the epoxypentane and the like, which are relatively low in activity, low in reaction yield and rate, results in poor final repair effect, and therefore, epoxybutane is preferable.
Preferably, the water-soluble linear diamine, the epoxy compound, and the remaining components are stored separately. The water-soluble linear diamine and the epoxy compound are liquid in the conventional state, and thus are not suitable for mixing with portland cement, while the nano silica and the hydroxyapatite are solid in the conventional state, and therefore, even if they are mixed with portland cement, the final result is not affected.
It is known to those skilled in the art that, for conventional portland cement, the volume thereof is shrunk during hardening and forming, so that a certain microcrack is generated in the later stage of the set cement, because, in order to compensate for the volume shrinkage of the set cement, a corresponding light burned magnesia may be added, and for light burned magnesia, the size is required to be smaller than 60 μm, because the larger the size is, the slower the expansion speed is, and the inventor finds that when the size is smaller than 60 μm, the cement has a certain expansion performance in the earlier stage, and can compensate for the hardening shrinkage in the earlier stage of the set cement. The addition amount of the light burned magnesia is 1-1.5% of the addition amount of the silicate cement by mass percent. Preferably, the addition amount of the light burned magnesia is 1.2% of the addition amount of the silicate cement.
The self-repairing cement system resistant to carbon dioxide corrosion is used for sealing an environment with high-pressure carbon dioxide, wherein the high-pressure carbon dioxide refers to carbon dioxide with the pressure or partial pressure of more than 5MPa. When in use, silicate cement is mixed according to a conventional method, and meanwhile, corresponding water-soluble linear diamine, epoxy compound, nano silicon dioxide, hydroxyapatite and light burned magnesia are added in the mixing process, and then the mixture is cured and formed according to the conventional method.
The beneficial effects of the invention are as follows: the self-repairing cement system can carry out self-repairing in a high-pressure carbon dioxide environment, has a good self-repairing effect, has a maximum 10d compressive strength recovery rate of more than 95%, has good self-repairing performance, and has a relatively high repairing speed; meanwhile, the self-repairing cement system has better carbon dioxide resistance, and the strength loss rate is about 11% at the minimum when the self-repairing cement system is completely placed in a high-pressure carbon dioxide environment for 90 days, so that the self-repairing cement system can resist carbon dioxide corrosion. In summary, the self-repairing cement system of the invention can be applied to high-pressure carbon dioxide environments, such as carbon dioxide underground gas reservoirs.
Detailed Description
In order to more clearly understand the technical features, objects and advantages of the present invention, the following detailed description of the technical solution of the present invention will be given with reference to examples, but should not be construed as limiting the scope of the present invention.
In the following examples, unless otherwise specified, the operations are those conventionally known in the art.
In the examples which follow, the starting materials are conventional commercial products in the art unless specifically stated otherwise.
In the following examples, the size of the light burned magnesium oxide was less than 60. Mu.m.
In the following examples, the following procedure was used to prepare the corresponding cement systems:
5kg of Portland cement is taken, water-soluble linear diamine, epoxy compound, hydroxy phosphorus lime and light burned magnesia shown in table 1 are taken at the same time, then standard sand and water with corresponding amounts are added and mixed evenly by adopting a method shown in GB/T17671-2021, and then curing molding is carried out.
Table 1 Material addition table
To further illustrate the self-healing effect that the self-healing cement systems prepared in the examples and comparative examples described above have, they are tested as follows.
1. Self-repairing performance test: the compressive strength was measured by the method described in GB/T17671-2021, and the final test results are shown in Table 2. Meanwhile, before the compressive strength of the steel is detected, the following maintenance is needed:
when the cement stone is cured for 28d, the cement stone is pre-pressed, the pre-pressing force is 60% of the compressive strength of 28d, after the pre-pressing is finished, the cement stone is placed in a carbon dioxide atmosphere, the pressure is 7MPa, and the cement stone is cured for 10d, and the compressive strength is tested during the curing. In order to meet the above setting, for the self-repairing cement system of the same formula, a plurality of self-repairing cement systems are required to be set at the same time, and curing and molding are required to be carried out under the same condition.
Table 2 compressive strength test results
From Table 2, it can be seen that the self-repairing cement system of the embodiment of the invention can effectively perform self-repairing when placed in a carbon dioxide atmosphere under a certain pressure condition, and the recovery rate of the 10d compressive strength can reach more than 95%.
Comparing the experimental results of example 1, example 2 and example 5, it was found that the selection of the water-soluble linear diamine had a certain effect on the final self-healing efficiency.
Comparing the experimental results of example 1 and example 3, it can be found that the selection of the epoxy compound has an influence on the self-repairing efficiency of the set cement, and also has a larger influence on the compressive strength of the set cement, probably because the propylene oxide adopted in example 3 has a lower boiling point, and is easy to undergo phase transition in the curing and forming process of the set cement, so that the set cement volatilizes. The volatilized propylene oxide not only can reduce the content of residual propylene oxide in the final set cement, but also can reduce the content of propylene oxide in the set cement relatively, so that the reaction rate and the product concentration of the set cement and high-pressure carbon dioxide are relatively low, and the self-repairing performance of the set cement is relatively reduced; meanwhile, when the epoxypropane is volatilized into gases, the gases can also generate certain air holes in the cement stone, and the strength of the cement stone can be reduced due to the existence of the air holes.
Comparing the experimental results of example 1 and example 4, it can be found that when no light-burned magnesia is added, the compressive strength and the compressive strength recovery rate of the cement stone are reduced to a certain extent, which is probably due to the fact that after the cement stone is pre-pressed, certain microcracks are generated, and the expansion effect of the light-burned magnesia can plug part of the microcracks to a certain extent, so that the compressive strength recovery rate of the cement stone can be increased.
Comparing the experimental results of example 1, example 6, example 7 and comparative example 5, it was found that the addition amount of each material had a certain effect on the final self-repairing effect of the set cement.
Comparing the experimental results of example 1, comparative example 1 and comparative example 2, it can be found that the nano silica and the hydroxyapatite have a certain influence on the compressive strength of the set cement.
In fact, although only the self-healing properties of the self-healing cement system of the examples of the present invention were tested in a carbon dioxide environment at a pressure of 7MPa, it was found through a number of experiments by the inventors that the self-healing cement system of the present invention can be applied in an environment at a pressure of more than 5MPa. When the pressure is lower than 7MPa, the lower the ambient pressure is, the slower the self-repairing speed is, and when the pressure exceeds 7MPa, the self-repairing speed is not changed greatly, and even in supercritical carbon dioxide, the self-repairing effect can be kept correspondingly.
2. Carbon dioxide tolerance test
The cement stone was prepared and cured by the method shown in GB/T17671-2021, then the formed cement stone was placed in a carbon dioxide atmosphere under a pressure of 7MPa, the compressive strength was measured after 90 days, and the final result was shown in Table 3, wherein the blank was Portland cement, without any additives, and the cement stone was prepared by the method shown in GB/T17671-2021, and after the curing formation, the curing was continued in the room for the same curing time as the rest of the cement stone.
TABLE 3 carbon dioxide Corrosion resistance test results
The intensity loss rate is calculated as follows
In which, in the process,/>
the compressive strength of the blank cement stone is MPa; b is the compressive strength of the cement stone to be tested after being corroded by carbon dioxide and MPa; n is the intensity loss rate,%.
As can be seen from table 3, even if the set cement according to the embodiment of the present invention is completely disposed in a high-pressure carbon dioxide environment, the strength loss rate is relatively small and can reach 11% at the minimum, and since the test is an extreme environment of the test, that is, the set cement is completely exposed to the high-pressure carbon dioxide environment, in the actual production process, only part (one or both sides) of the set cement is usually contacted with the high-pressure carbon dioxide, and the carbon dioxide only corrodes the contact surface; and the cement stone is relatively thick in whole, so that the cement stone has relatively better effect and lower strength loss rate when being applied to the actual environment. And referring to comparative examples 1-5, the raw materials and the addition amount of the raw materials in the invention have great influence on the carbon dioxide corrosion resistance of the cement stone.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the technical scope of the present invention disclosed in the embodiments of the present invention should be covered by the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (6)
1. The self-repairing cement system resistant to carbon dioxide corrosion is characterized by comprising Portland cement, water-soluble linear diamine, an epoxy compound, nano silicon dioxide and hydroxyapatite, wherein the water-soluble linear diamine accounts for 1-2% of the Portland cement, the epoxy compound accounts for 0.3-1.5% of the Portland cement, the nano silicon dioxide accounts for 1-3% of the Portland cement, and the hydroxyapatite accounts for 1-2.5% of the Portland cement.
2. The carbon dioxide corrosion resistant self-healing cement system according to claim 1, wherein the water soluble linear diamine is one of ethylenediamine, 1, 4-butanediamine, 1, 5-pentanediamine, hexamethylenediamine; the epoxy compound is butylene oxide.
3. The carbon dioxide corrosion resistant self-healing cement system according to claim 2, wherein the water soluble linear diamine is 1, 4-butanediamine.
4. A self-healing cement system resistant to carbon dioxide corrosion according to any one of claims 1 to 3, wherein the water-soluble linear diamine, epoxy compound are stored separately from the remaining components.
5. The carbon dioxide corrosion resistant self-repairing cement system according to claim 1, further comprising light burned magnesia, wherein the size of the light burned magnesia is smaller than 60 μm, and the addition amount of the light burned magnesia is 1-1.5% of the addition amount of the Portland cement in percentage by mass.
6. The carbon dioxide corrosion resistant self-repairing cement system according to claim 1, wherein the water-soluble linear diamine is 1.4-1.6% of the Portland cement, the epoxy compound is 0.8-1.0% of the Portland cement, the nano silicon dioxide is 1.8-2.2% of the Portland cement, and the hydroxyapatite is 1.6-2.0% of the Portland cement in percentage by mass.
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