CN117820667A - Environment-friendly heat-resistant water-based drilling fluid additive and preparation method and application thereof - Google Patents
Environment-friendly heat-resistant water-based drilling fluid additive and preparation method and application thereof Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 238000005553 drilling Methods 0.000 title claims abstract description 104
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- 239000000654 additive Substances 0.000 title claims abstract description 83
- 230000000996 additive effect Effects 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000002639 bone cement Substances 0.000 claims abstract description 71
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 45
- 241001465754 Metazoa Species 0.000 claims abstract description 37
- PAAZPARNPHGIKF-UHFFFAOYSA-N 1,2-dibromoethane Chemical compound BrCCBr PAAZPARNPHGIKF-UHFFFAOYSA-N 0.000 claims abstract description 36
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- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical group CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 9
- 238000005904 alkaline hydrolysis reaction Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 241000219053 Rumex Species 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 abstract description 26
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- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 0.000 description 34
- 229940080314 sodium bentonite Drugs 0.000 description 34
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 4
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
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Abstract
The invention discloses an environment-friendly temperature-resistant water-based drilling fluid additive, a preparation method of the environment-friendly temperature-resistant water-based drilling fluid additive and application of the environment-friendly temperature-resistant water-based drilling fluid additive to drilling fluid, wherein the preparation method of the environment-friendly temperature-resistant water-based drilling fluid additive comprises the following steps of: the animal bone glue is used as a raw material, 1, 2-dibromoethane is used as a modifier, etherification reaction is carried out, the pH value of the system is regulated by sodium hydroxide, and a chain transfer agent is added to accurately control the molecular weight of the polymer, so that the additive is finally obtained. The invention realizes the modification of the easily-decomposed environment-friendly macromolecular substance animal bone glue, so that the animal bone glue can be used as a shale inhibitor to be applied to drilling fluid, and has higher environment-friendly performance; the heat stability is good, the inhibition is good, the heat stabilizer can be directly used in water-based drilling fluid, and the defects that the inhibition rate of the conventional shale inhibitor in the oil field is still to be improved, the temperature resistance is poor, the environmental acceptability is weak and the like are overcome.
Description
Technical Field
The invention relates to the field of drilling fluid additives, in particular to an environment-friendly temperature-resistant water-based drilling fluid additive, and a preparation method and application thereof.
Background
The deep oil gas resource in China has wide distribution range and large reserves, becomes a main backup energy for relieving the contradiction between energy supply and demand in China, and is a great guarantee for national energy safety. The drilling fluid is the 'blood' of the drilling engineering, and is a key technology for preventing malignant accidents such as collapse, sticking, lost circulation, blowout and the like in the deep well drilling process.
In the process of developing deep well oil gas resources, in order to solve the problem of common drilling accidents in deep well drilling operation of well wall instability, shale inhibitors are added into drilling fluid in the prior art, so that hydration dispersion of shale can be slowed down to a certain extent, and well wall stability is maintained.
At present, the deep well temperature-resistant drilling fluid is mainly a polysulfonate drilling fluid system developed in seventies of the last century, but in deep well drilling, polymer additives in the drilling fluid are easy to decompose when the temperature rises, the inhibiting effect is lost, the performance of the drilling fluid is deteriorated, mud and shale are hydrated and expanded due to the failure of the drilling fluid, and the well wall is unstable.
And the polysulfonate drilling fluid is difficult to degrade into harmless substances, and has poor environmental protection performance. Along with the gradual strictness of national requirements on environmental protection, the development of temperature-resistant environmental-friendly drilling fluid treatment agents is urgent, the high-temperature-resistant drilling fluid technology faces unprecedented significant challenges, and the technology belongs to the leading-edge subject of the drilling field at home and abroad.
Based on the above, it is of great significance to explore a drilling fluid additive which is environment-friendly, temperature-resistant and not easy to age.
Disclosure of Invention
The invention aims to provide an environment-friendly temperature-resistant water-based drilling fluid additive, a preparation method and application thereof, and aims to solve the technical problems that the inhibition rate performance of shale inhibitors is still to be improved and the temperature resistance is poor in the prior art.
In order to solve the technical problems, the invention specifically provides the following technical scheme:
the invention provides an environment-friendly heat-resistant water-based drilling fluid additive, which has a structural formula shown in a structural formula (I):
wherein,represents a peptide bond, n=75-90.
As a preferred embodiment of the present invention, the additive is bone cement modified by 1, 2-dibromoethane.
The invention provides a preparation method of an environment-friendly temperature-resistant water-based drilling fluid additive, which comprises the following steps:
the animal bone glue is used as a raw material, and 1, 2-dibromoethane is used as a modifier to carry out etherification reaction, so that the additive is obtained.
As a preferred embodiment of the present invention, the method comprises the steps of:
adding water into the animal bone glue, and fully dissolving for 10-18 hours at normal temperature to obtain glue solution with viscoelasticity;
adding sodium hydroxide into the glue solution, and performing alkaline hydrolysis at the water bath temperature of 60-70 ℃ to obtain a reaction solution;
sequentially adding 1, 2-dibromoethane and a chain transfer agent into the reaction liquid, and heating and refluxing to obtain a mixed product;
purifying and drying the mixed product to obtain the additive;
the reaction formula of the environment-friendly heat-resistant water-based drilling fluid additive, namely the 1, 2-dibromoethane modified bone cement, is as follows:
as a preferable scheme of the invention, the mass ratio of the animal bone glue to the water is 1:1-1:1.5;
wherein the mass ratio of the glue solution to the 1, 2-dibromoethane is 70:1;
wherein the mass ratio of the sodium hydroxide to the 1, 2-dibromoethane is 1:2-2:1;
wherein the chain transfer agent accounts for 0.05-0.15% of the mass of the glue solution.
As a preferred embodiment of the present invention, the chain transfer agent is dodecyl mercaptan.
As a preferred embodiment of the present invention, the alkaline hydrolysis satisfies the following conditions: stirring for 0.5-1.5 h at 60-70 ℃;
the heating reflux meets the following conditions: the stirring time is 2-6 h, and the stirring temperature is 50-60 ℃.
As a preferable scheme of the invention, the bone glue is bovine bone glue;
wherein the bovine bone glue comprises any one or more of Mongolian cattle, qinchuan cattle, nanyang cattle and Rumex cattle.
The invention provides an application of an additive in environment-friendly heat-resistant water-based drilling fluid.
As a preferred aspect of the present invention, the additive, when added to a drilling fluid, serves to retard the rate of decomposition of the drilling fluid.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the problem that the environment-friendly polymer animal bone glue is free from water invasion and can be reduced in cohesiveness due to dissolution in a large amount of water can be solved by the 1, 2-dibromoethane modified polymer bone glue, so that the polymer bone glue is changed into a stable polymer, the hydrophobicity and the temperature resistance are improved to a large extent, the application range of the animal bone glue is widened, and the shale inhibitor has environment-friendly performance;
through experimental tests, the modified product has excellent shale inhibition effect and good thermal stability even after aging at 130 ℃; the shale inhibition effect of the shale is higher than that of KCl which is a commonly used inhibitor in oil fields; the product is easy to dissolve in water, can be directly used in water-based drilling fluid, and solves the defects that the inhibition rate performance of the conventional shale inhibitor in the oil field is still to be improved, the temperature resistance is poor, the environmental acceptability is weak and the like;
the invention is that the glue solution after the animal bone glue is fully dissolved in water is mixed with 1, 2-dibromoethane according to a certain proportion, and under the effect of sodium hydroxide alkaline hydrolysis, chain transfer agent is added to carry out etherification reaction, the reaction mode can accurately control the polymerization degree of polymer products between 75 and 90, thereby obtaining modified bone glue with target molecular weight, and solving the technical defect that the molecular weight cannot be controlled manually; meanwhile, the problem of non-water invasion resistance of bone glue is solved, and the rheological property of drilling fluid is not influenced while the inhibition effect is obvious;
the preparation method has the advantages of simple and convenient preparation steps, relatively mild reaction conditions, low cost, readily available raw materials of the components required during the preparation and easy application to industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It will be apparent to those of ordinary skill in the art that the drawings in the following description are exemplary only and that other implementations can be obtained from the extensions of the drawings provided without inventive effort.
FIG. 1 is an infrared spectrum of a glue solution after dissolution of animal bone glue (before modification with 1, 2-dibromoethane) used in example 5;
FIG. 2 is an infrared spectrum of the environmental protection heat-resistant water-based drilling fluid additive in example 5 prepared by the invention;
FIG. 3 is an XRD pattern of an example 5 environmental protection and temperature resistance water-based drilling fluid additive prepared by the invention before and after addition of base slurry.
FIG. 4 is a statistical plot of the effect of base slurry containing varying concentrations of the environment-friendly, temperature-resistant water-based drilling fluid additive of example 5 prepared according to the present invention on the linear expansion rate of sodium bentonite.
FIG. 5 is a statistical plot of the effect of the base slurry prepared according to the invention containing the example 5 environmentally friendly temperature resistant water-based drilling fluid additive on the linear expansion rate of sodium bentonite at different temperatures.
FIG. 6 is a graph showing the linear expansion coefficient of a base slurry containing 5% of the environment-friendly and temperature-resistant water-based drilling fluid additive of example 5 prepared according to the present invention after being added to sodium bentonite, compared with a base slurry containing 6% of the inhibitor KCl commonly used in oil fields of comparative example 1 after being added to sodium bentonite.
FIG. 7 is a statistical plot of the effect of base slurry containing varying concentrations of the environment-friendly, temperature-resistant water-based drilling fluid additive of example 1 prepared according to the present invention on the linear expansion rate of sodium bentonite.
FIG. 8 is a statistical plot of the effect of base slurry containing varying concentrations of the environment-friendly, temperature-resistant water-based drilling fluid additive of example 2 prepared according to the present invention on the linear expansion rate of sodium bentonite.
FIG. 9 is a statistical plot of the effect of base slurry containing varying concentrations of the environment-friendly, temperature-resistant water-based drilling fluid additive of example 3 prepared according to the present invention on the linear expansion rate of sodium bentonite.
FIG. 10 is a statistical plot of the effect of base slurry containing varying concentrations of the environment-friendly, temperature-resistant water-based drilling fluid additive of example 4 prepared according to the present invention on the linear expansion coefficient of sodium bentonite.
FIG. 11 is a statistical plot of the effect of base slurry containing varying concentrations of the example 6 environmental protection, temperature resistant water-based drilling fluid additive prepared according to the present invention on the linear expansion rate of sodium bentonite.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As a degradable natural high molecular polymer, the animal bone glue has the advantages of strong toughness, high elasticity, low cost, environmental protection and convenient use, and can be applied to drilling fluid through analyzing the properties of the animal bone glue. However, after intensive research, it was found that it is not water-invasion resistant, is soluble in a large amount of water, causes a decrease in cohesiveness, and has not been reported in oilfield chemistry at present, and has not been a precedent for application in drilling fluids.
In order to improve the performance of animal bone glue and enable the animal bone glue to be stably applied to drilling fluid, the invention provides an environment-friendly heat-resistant water-based drilling fluid additive which is used for being added into the drilling fluid to maintain the stability of the drilling fluid.
Specifically, the structural formula of the additive is shown as structural formula (I):
wherein the method comprises the steps ofRepresents a peptide bond, n=75-90.
The polymer is prepared from animal bone glue and 1, 2-dibromoethane through etherification reaction, namely 1, 2-dibromoethane modified bone glue Abg.
In the invention, animal bone glue is used as a raw material, and is modified by 1, 2-dibromoethane to be changed into a stable polymer, so that the hydrophobicity and the temperature resistance of the modified bone glue are improved to a greater extent, and the modified bone glue is expected to be applied to oilfield chemistry as a temperature-resistant environment-friendly shale inhibitor.
The invention introduces bone cement which is excellent in temperature resistance and is not applied in oilfield chemistry and is derived from bovine bone into the drilling fluid industry, so as to research an environment-friendly temperature-resistant water-based drilling fluid additive. Through experimental tests, the shale inhibition effect of the modified product is excellent even after aging at 130 ℃.
Furthermore, the invention provides a preparation method of the environment-friendly heat-resistant water-based drilling fluid additive, which is prepared by adding animal bone glue into 1, 2-dibromoethane and carrying out etherification reaction.
In the reaction process, the molecular weight of the polymer cannot be controlled artificially, if the molecular weight is too large, the fluidity of the polymer is changed, the drilling fluid becomes viscous after the polymer is added into the drilling fluid, and if the molecular weight is too small, the reaction is failed.
In order to accurately control the polymerization degree to be 75-90 and obtain the modified bone glue with target molecular weight, chain transfer agent is added into reaction liquid through distributed reaction in the reaction process, so that the accurate control of the polymerization degree is realized, and the technical defect that the molecular weight of the polymer cannot be controlled manually is overcome.
Specifically, the method comprises the following steps:
dissolving: fully dissolving animal bone glue and water at normal temperature for 10-18 h to form a viscoelasticity glue solution;
alkaline hydrolysis: then, the glue solution is drained into a round-bottom flask, a small amount of sodium hydroxide is added into the flask, the flask is reacted in a water bath environment, and the reaction is stirred at the temperature to obtain a reaction solution;
and (3) heating and refluxing: then adding 1, 2-dibromoethane under the reaction condition, adding a small amount of chain transfer agent into the system, accurately controlling the molecular weight of the reaction system, stirring the reaction while cooling to a certain temperature, and reacting the reaction at the temperature to obtain a mixed product;
purifying and drying: and taking out the mixed product in the flask after the reaction is finished, and purifying and fully drying to obtain the environment-friendly heat-resistant water-based drilling fluid additive.
Sequentially adding 1, 2-dibromoethane and a chain transfer agent into the reaction liquid, and heating and refluxing to obtain a mixed product;
purifying and drying the mixed product to obtain the additive.
The reaction formula of the environment-friendly heat-resistant water-based drilling fluid additive, namely the 1, 2-dibromoethane modified bone cement, is as follows:
the synthetic product Abg is obtained by etherification reaction of glue solution of animal bone glue fully dissolved in water and 1, 2-dibromoethane according to a certain proportion under the action of sodium hydroxide alkaline hydrolysis, and the polymerization degree of the polymer can be precisely controlled between 75 and 90 by the reaction mode, so that the modified bone glue with target molecular weight is obtained, and the technical defect that the molecular weight cannot be controlled manually is overcome. Meanwhile, the problem of non-water invasion resistance of bone glue is solved, and the inhibition effect is obvious and the rheological property of drilling fluid is not affected.
The preparation method has the advantages of simple and convenient preparation steps, mild reaction conditions, low cost, readily available raw materials of other components and applicability to industrial production.
Further, in a preferred embodiment, the mass ratio of the animal bone glue to the water is 1:1 to 1:1.5, more preferably, the mass ratio of the animal bone glue to the water is 1:1.
In a preferred embodiment, the mass ratio of the gum solution to the 1, 2-dibromoethane is 70:1.
In a preferred embodiment, the mass ratio of the sodium hydroxide to the 1, 2-dibromoethane is 1:2-2:1.
In a preferred embodiment, the chain transfer agent comprises 0.05 to 0.15% by weight of the gum solution.
In a preferred embodiment, the chain transfer agent is dodecyl mercaptan.
In a preferred embodiment, the alkaline hydrolysis satisfies the following conditions: the stirring time is 0.5-1.5 h, the stirring temperature is 60-70 ℃, and the optimal stirring temperature is 70 ℃.
In a preferred embodiment, the heated reflux meets the following conditions: the stirring time is 2-6 h, and the stirring temperature is 50-60 ℃.
In a preferred embodiment, the bone glue is bovine bone glue, more preferably, the bovine bone glue comprises any one or more of Mongolian cows, qinchuan cattle, nanyang cows and Rumex.
When the water-based drilling fluid additive is applied to the drilling fluid as a shale inhibitor, the addition amount of the water-based drilling fluid additive is 1-5% based on the mass of water in a configured drilling fluid system. The drilling fluid comprises clear water, lime soil and anhydrous sodium carbonate.
The environment-friendly and temperature-resistant water-based drilling fluid additive is further described below by way of specific examples.
All the starting materials and solvents used in the examples were commercially available products of the corresponding purity.
The bone glue is Mongolian bovine bone glue purchased from Henan Kaier chemical products Co., ltd, and is an industrial grade product.
Example 1
Fully dissolving animal bone glue and water for 10 hours at normal temperature according to the mass ratio of 1:1;
adding the dissolved glue solution into a round-bottom flask through drainage, then adding 0.5g of sodium hydroxide, and stirring the flask for 0.5h in a water bath environment at 70 ℃;
then 1g of 1, 2-dibromoethane is added into the flask, then 0.05 percent (the specific weight of the mass of the glue solution) of dodecyl mercaptan is added, the water bath temperature is reduced to 55 ℃ while the reaction is stirred, and the reaction is carried out for 2 hours through condensation and reflux;
and after the reaction is finished, purifying and fully drying the product in the flask to obtain the temperature-resistant environment-friendly water-based drilling fluid additive. The degree of polymerization of the polymer at this time was 77.
Example 2
Fully dissolving animal bone glue and water for 12 hours at normal temperature according to the mass ratio of 1:1;
adding the dissolved glue solution into a round-bottom flask through drainage, then adding 0.5g of sodium hydroxide, and stirring the flask for 1h in a water bath environment at 70 ℃;
then adding 1g of 1, 2-dibromoethane, then adding 0.05 percent (the specific weight of the mass of the glue solution) of dodecyl mercaptan, reducing the water bath temperature to 55 ℃ while stirring the reaction, and carrying out condensation reflux reaction for 3 hours;
and after the reaction is finished, purifying and fully drying the product in the flask to obtain the temperature-resistant environment-friendly water-based drilling fluid additive. The degree of polymerization of the polymer at this time was 79.
Example 3
Fully dissolving animal bone glue and water for 14h at normal temperature according to the mass ratio of 1:1.1;
adding the dissolved glue solution into a round-bottom flask through drainage, then adding 1g of sodium hydroxide, and stirring the flask for 1h in a water bath environment at 60 ℃;
then adding 1g of 1, 2-dibromoethane, then adding 0.1 percent (the specific weight of the mass of the glue solution) of dodecyl mercaptan, stirring the reaction, reducing the water bath temperature to 50 ℃, and carrying out condensation reflux reaction for 4 hours;
and after the reaction is finished, purifying and fully drying the product in the flask to obtain the temperature-resistant environment-friendly water-based drilling fluid additive. The degree of polymerization of the polymer at this time was 82.
Example 4
Fully dissolving animal bone glue and water for 16 hours at normal temperature according to the mass ratio of 1:1.3;
adding the dissolved glue solution into a round-bottom flask through drainage, then adding 1g of sodium hydroxide, and stirring the flask for 0.5h in a water bath environment at 60 ℃;
then adding 1.2g of 1, 2-dibromoethane, then adding 0.1 percent (the specific weight of the mass of the glue solution) of dodecyl mercaptan, reducing the water bath temperature to 50 ℃ while stirring the reaction, and carrying out condensation reflux reaction for 6 hours;
and after the reaction is finished, purifying and fully drying the product in the flask to obtain the temperature-resistant environment-friendly water-based drilling fluid additive. The degree of polymerization of the polymer at this time was 79.
Example 5
Fully dissolving animal bone glue and water for 18 hours at normal temperature according to the mass ratio of 1:1;
adding the dissolved glue solution into a round-bottom flask through drainage, then adding 1g of sodium hydroxide, and stirring the flask for 0.5h in a water bath environment at 70 ℃;
then 0.5g of 1, 2-dibromoethane is added, then 0.12 percent (the specific weight of the mass of the glue solution) of dodecyl mercaptan is added, the water bath temperature is reduced to 60 ℃ while the reaction is stirred, and the condensation reflux reaction is carried out for 4 hours;
and after the reaction is finished, purifying and fully drying the product in the flask to obtain the temperature-resistant environment-friendly water-based drilling fluid additive. The degree of polymerization of the polymer at this time was 80.
Example 6
Fully dissolving animal bone glue and water for 18h at normal temperature according to the mass ratio of 1:1.5;
adding the dissolved glue solution into a round-bottom flask through drainage, then adding 1g of sodium hydroxide, and stirring the flask for 0.5h in a water bath environment at 60 ℃;
then 0.5g of 1, 2-dibromoethane is added, then 0.15 percent (the specific weight of the mass of the glue solution) of dodecyl mercaptan is added, the water bath temperature is reduced to 60 ℃ while the reaction is stirred, and the condensation reflux reaction is carried out for 6 hours;
and after the reaction is finished, purifying and fully drying the product in the flask to obtain the temperature-resistant environment-friendly water-based drilling fluid additive. The degree of polymerization of the polymer at this time was 82.
To evaluate the inhibitory effect of the present product, the product obtained by the synthesis method in example 5 was subjected to the following analysis:
1. infrared analysis
The products before and after synthesis in example 5 were taken, a small amount of sample was sucked and placed on a sample holder for testing by using a Brookfield infrared spectrometer.
The infrared absorption spectrum diagrams of the glue solution before and after the modification of the 1, 2-dibromoethane are shown in fig. 1 and 2, the infrared absorption spectrum diagram of the glue solution after the dissolution of the animal bone glue before the modification of the 1, 2-dibromoethane is shown in fig. 1, and the infrared absorption spectrum diagram of the environment-friendly heat-resistant water-based drilling fluid additive prepared by the invention is shown in fig. 2.
As can be seen from FIG. 1, at 3300cm -1 Near the expansion vibration peak, 1640cm -1 Bending vibration peak appears nearby, which indicates that-NH exists in bone glue 2 。
As can be seen from FIG. 2, at 3300cm -1 ，2800cm -1 The vicinity is the stretching vibration peak of O-H bond in carboxylic acid; at 1700cm -1 A stretching vibration peak with c=o bond nearby; 1350cm -1 An absorption peak appears, indicating that-OH exists in the modified bone glue; a stretching vibration peak appears near 1030cm < -1 >, which indicates that C-O bonds exist in the modified bone glue; at 690cm -1 Bending vibration peaks appear nearby, indicating the presence of C-Br bonds in the modified bone glue.
The animal bone glue is not decomposed into small molecules in the reaction process of the animal bone glue and the 1, 2-dibromoethane, the reaction achieves the aim of combining the animal bone glue and the 1, 2-dibromoethane, and the performance of the animal bone glue against water invasion is improved.
The result shows that the environment-friendly and temperature-resistant modified bone glue is successfully synthesized.
2. XRD analysis experiment
(1) Two groups of 350mL base slurry (clear water, lime soil and anhydrous sodium carbonate) are taken and respectively placed in 500mL beakers, one group is used as a blank control, and the other group is added with the polymer synthesized in the example 5 with the concentration of 5 percent, and the mixture is stirred at a high speed for 30 minutes, so that the polymer synthesized by the invention and the base slurry are fully and uniformly mixed.
(2) Pouring the two groups of samples into a centrifugal cup, centrifuging for 20min after the centrifugal machine is set at 4000 rpm, pouring out supernatant, placing residual slurry into a clean surface dish, drying for 24h at 120 ℃ in an oven until the dry block is free of moisture, taking out the samples, pouring the samples into a mortar for grinding, and repeatedly sieving with a screen to obtain the required samples.
(3) The sample was subjected to XRD testing with a scan range 2θ=5 to 80 °, and a scan speed of 10 °/min.
As shown in FIG. 3, FIG. 3 is an XRD pattern of the environment-friendly and temperature-resistant water-based drilling fluid additive of example 5 before and after the addition of the base slurry, which shows that the XRD pattern of the base slurry before and after the addition of the environment-friendly and temperature-resistant water-based drilling fluid additive has smaller peak or overlaps other peaks although the corresponding peaks appear, because of the possible presence of SiO 2 The characteristic peak is too strong, and the like, and the main functional group of the indirect product is adsorbed in the base slurry, so that the adsorption effect is obvious.
3. Linear expansion experiment
(1) Taking 8+/-0.01 g of 100 mesh sodium bentonite which is dried for 4 hours at 100+/-5 ℃ and cooled to room temperature, and placing the bentonite in a measuring cylinder;
(2) After pressing for 5min at 10MPa on a press, taking out a plug rod, taking out a pressed sheet, and measuring the thickness of the rock core by using a vernier caliper;
(3) Based on the mass of water in a matrix system, the matrix containing 0 percent (pure matrix), 1 percent, 2 percent, 3 percent, 4 percent and 5 percent of the water-based drilling fluid additive prepared in the example 5 is poured into a measuring cylinder, a normal temperature and normal pressure linear expansion instrument is adopted in the experiment, and the linear expansion rate is measured by recording readings at different moments.
The test results are shown in fig. 4, and fig. 4 is a statistical graph of the effect of base slurry containing different concentrations of the environment-friendly temperature-resistant water-based drilling fluid additive prepared in example 5 of the present invention on the linear expansion rate of sodium bentonite.
When only pure base paddles, namely the water-based drilling fluid additive with the concentration of 0 percent, are added, the final linear expansion rate of the sodium bentonite is 51.2 percent;
the linear expansion rate of sodium bentonite was 49.9% upon addition of a base slurry containing 1% of the water-based drilling fluid additive prepared in example 5;
the linear expansion rate of sodium bentonite was 42.9% upon addition of a base slurry containing 2% of the water-based drilling fluid additive prepared in example 5;
the linear expansion rate of sodium bentonite was 38.6% with the addition of a base slurry containing 3% of the water-based drilling fluid additive prepared in example 5;
the linear expansion rate of sodium bentonite was 34.9% with the addition of a base slurry containing 4% of the water-based drilling fluid additive prepared in example 5;
from the experimental results, it is found that the linear expansion rate of the sodium bentonite containing the additive of the present invention is reduced by 29.7% relative to the sodium bentonite containing only the base slurry after 5% of the water-based drilling fluid additive prepared in example 5 is added to the base slurry. This indicates that the additive has good inhibition to the base slurry. The additive disclosed by the invention is added into the drilling fluid, so that the inhibition of the drilling fluid can be improved, the hydration dispersion degree of shale can be effectively relieved, and the stability of a well wall can be maintained.
4. Temperature resistance experiment
(1) Taking 8+/-0.01 g of 100 mesh sodium bentonite which is dried for 4 hours at 100+/-5 ℃ and cooled to room temperature, and placing the bentonite in a measuring cylinder;
(2) After pressing for 5min at 10MPa on a press, taking out a plug rod, taking out a pressed sheet, and measuring the thickness of the rock core by using a vernier caliper;
(3) Based on the mass of water in the drilling fluid system, the base slurry containing 5% of the water-based drilling fluid additive prepared in example 5 is poured into a measuring cylinder, and the linear expansion rate is measured by recording readings of different temperatures by using a normal temperature and normal pressure linear expansion instrument in the experiment, wherein the temperature ranges are 100 ℃, 110 ℃, 120 ℃ and 130 ℃.
The test results are shown in fig. 5, fig. 5 shows the linear expansion rate of sodium bentonite at different temperatures after the base slurry is added into the environment-friendly temperature-resistant water-based drilling fluid additive of the embodiment 5 prepared by the invention, and fig. 5 shows the influence of temperature on the linear expansion rate of the sodium bentonite added with the product.
As shown in FIG. 5, the linear expansion rate of sodium bentonite after adding the base slurry containing 5% of example 5 at 100℃was 28.6%;
at 110 ℃, the linear expansion rate of the sodium bentonite is 29.3% after the sodium bentonite is added into the base slurry containing 5% of the example 5;
at 120 ℃, the linear expansion rate of the sodium bentonite is 29.7% after the sodium bentonite is added into the base slurry containing 5% of the example 5;
at 130℃the linear expansion of the sodium bentonite after addition of the 5% base slurry of example 5 was 33.1%.
The result shows that the product still shows good inhibition on the base slurry at 130 ℃, and the temperature has little influence on the additive prepared by the invention.
The excellent properties of the additives of the present invention are demonstrated by the comparative examples below.
5. Comparative example experiment
Comparative example 1
(1) Taking 8+/-0.01 g of 100 mesh sodium bentonite which is dried for 4 hours at 100+/-5 ℃ and cooled to room temperature, and placing the bentonite in a measuring cylinder;
(2) After pressing for 5min at 10MPa on a press, taking out a plug rod, taking out a pressed sheet, and measuring the thickness of the rock core by using a vernier caliper;
(3) Based on the mass of water in the base slurry, adding a common inhibitor KCl in an oil field into the base slurry, wherein the concentration is 6%, pouring the base slurry containing the inhibitor into a measuring cylinder, adopting a normal temperature and normal pressure linear expansion instrument for experiments, and measuring the linear expansion rate by recording readings of different temperatures.
The linear expansion coefficient of the sodium bentonite in the above comparative example 1 was also compared with that of the sodium bentonite containing 5% of the additive-based slurry of the invention of example 5 in the above linear expansion test, and the results are shown in fig. 6.
FIG. 6 is a graph showing the linear expansion coefficient of a base slurry containing 5% of the environment-friendly and temperature-resistant water-based drilling fluid additive of example 5 prepared according to the present invention after being added to sodium bentonite, compared with a base slurry containing 6% of the inhibitor KCl commonly used in oil fields of comparative example 1 after being added to sodium bentonite.
6. Verification experiments of other examples
(1) Taking 8+/-0.01 g of 100 mesh sodium bentonite which is dried for 4 hours at 100+/-5 ℃ and cooled to room temperature, and placing the bentonite in a measuring cylinder;
(2) After pressing for 5min at 10MPa on a press, taking out a plug rod, taking out a pressed sheet, and measuring the thickness of the rock core by using a vernier caliper;
(3) Based on the mass of water in the system of the configured base paddles, the base paddles containing 0 percent (pure base paddles), 1 percent, 2 percent, 3 percent, 4 percent and 5 percent of the water-based drilling fluid additive prepared in the example 1, the example 2, the example 3, the example 4 and the example 6 are respectively poured into a measuring cylinder, and the linear expansion rate is measured by recording readings at different moments by using a normal temperature and normal pressure linear expansion instrument in an experiment.
The recorded expansion rate charts are shown in fig. 7 to 11.
As shown in fig. 7 to 11, it was confirmed that examples 1,2, 3, 4 and 6 all showed similar properties to example 5, i.e., inhibition of the expansion rate of sodium bentonite in the linear expansion test after mixing with the base slurry, and thus it was found that the other examples were all successful 1, 2-dibromoethane-modified polymer bone cements.
The environment-friendly water-based drilling fluid additive can solve the problem that animal bone glue is not water-invasion-resistant and can be dissolved in a large amount of water to cause the adhesiveness to be reduced, and the animal bone glue is modified by 1, 2-dibromoethane to be changed into a stable polymer, so that the hydrophobicity and the temperature resistance are improved to a great extent, and the environment-friendly water-based drilling fluid additive is expected to be used as a shale inhibitor with temperature resistance and environment protection; through experimental tests, the modified product has excellent shale inhibition effect even after aging at 130 ℃, and the shale inhibition effect is higher than that of the KCl inhibitor commonly used in oil fields by 6%.
The preparation method of the environment-friendly heat-resistant water-based drilling fluid additive can accurately control the polymerization degree of the polymer to be 75-90, so that the modified bone cement with the target molecular weight is obtained, and the technical defect that the molecular weight cannot be controlled manually is overcome. Meanwhile, the preparation method solves the problem that bone glue is free of water invasion resistance, has obvious inhibition effect, does not have any influence on rheological property of drilling fluid, is simple and convenient in preparation step, mild in reaction condition and low in cost, and can be used for industrial production, and other component raw materials are easy to obtain.
The above embodiments are only exemplary embodiments of the present application and are not intended to limit the present application, the scope of which is defined by the claims. Various modifications and equivalent arrangements may be made to the present application by those skilled in the art, which modifications and equivalents are also considered to be within the scope of the present application.
Claims (9)
1. The environment-friendly heat-resistant water-based drilling fluid additive is characterized in that the structural formula of the additive is shown as structural formula (I):
wherein,represents a peptide bond, n=75-90.
2. The environment-friendly and temperature-resistant water-based drilling fluid additive as claimed in claim 1, wherein,
the additive is bone glue modified by 1, 2-dibromoethane.
3. A method for preparing the environment-friendly temperature-resistant water-based drilling fluid additive as claimed in any one of claims 1 to 2, comprising the following steps:
the animal bone glue is used as a raw material, and 1, 2-dibromoethane is used as a modifier to carry out etherification reaction, so that the additive is obtained.
4. The method for preparing the environment-friendly and temperature-resistant water-based drilling fluid additive as claimed in claim 3, which is characterized by comprising the following steps:
adding water into the animal bone glue, and fully dissolving for 10-18 hours at normal temperature to obtain glue solution with viscoelasticity;
adding sodium hydroxide into the glue solution, and performing alkaline hydrolysis at the water bath temperature of 60-70 ℃ to obtain a reaction solution;
sequentially adding 1, 2-dibromoethane and a chain transfer agent into the reaction liquid, and heating and refluxing to obtain a mixed product;
purifying and drying the mixed product to obtain the additive.
5. The method for preparing the environment-friendly and temperature-resistant water-based drilling fluid additive according to claim 3, wherein the method comprises the following steps of,
the mass ratio of the animal bone glue to the water is 1:1-1:1.5;
wherein the mass ratio of the glue solution to the 1, 2-dibromoethane is 70:1;
wherein the mass ratio of the sodium hydroxide to the 1, 2-dibromoethane is 1:2-2:1;
wherein the chain transfer agent accounts for 0.05-0.15% of the mass of the glue solution.
6. The method for preparing the environment-friendly and temperature-resistant water-based drilling fluid additive according to claim 3, wherein the method comprises the following steps of,
the chain transfer agent is dodecyl mercaptan.
7. The method for preparing the environment-friendly and temperature-resistant water-based drilling fluid additive according to claim 3, wherein the method comprises the following steps of,
the alkaline hydrolysis satisfies the following conditions: stirring for 0.5-1.5 h at 60-70 ℃;
the heating reflux meets the following conditions: the stirring time is 2-6 h, and the stirring temperature is 50-60 ℃.
8. The method for preparing the environment-friendly and temperature-resistant water-based drilling fluid additive according to claim 3, wherein the method comprises the following steps of,
the bone glue is bovine bone glue;
wherein the bovine bone glue comprises any one or more of Mongolian cattle, qinchuan cattle, nanyang cattle and Rumex cattle.
9. Use of the additive of claim 1 in a water-based drilling fluid.
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