CN115895611A - Amino polymer inhibitor for drilling fluid and preparation method thereof - Google Patents
Amino polymer inhibitor for drilling fluid and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of inhibitors for drilling fluid, and discloses an amino polymer inhibitor for drilling fluid and a preparation method thereof, wherein the inhibitor comprises the following raw materials in parts by weight: 40-80 parts of main inhibitor and 10-25 parts of auxiliary inhibitor, wherein the main inhibitor is prepared by taking acrylamide, acrylic acid, 2-acrylamido-2-methylpropanesulfonic acid, N- (3-aminopropyl) methacrylate and hydrochloride as polymerization monomers, and an oxidation reduction system consisting of sodium bisulfite and sodium persulfate as an initiator solution through free radical polymerization, and the auxiliary inhibitor is prepared by taking 3-chloropropionyl chloride, ethylene glycol and diethylenetriamine as raw materials; the composite amino polymer inhibitor has excellent performance of inhibiting hydration swelling of mineral clay by combining the dual inhibition effects of the primary inhibitor and the secondary inhibitor, and is beneficial to the application of the composite amino polymer inhibitor in drilling fluid.
Description
Technical Field
The invention relates to the technical field of inhibitors for drilling fluid, and in particular relates to an amino polymer inhibitor for drilling fluid and a preparation method thereof.
Background
The world-wide position of petroleum is self-evident, the reserves and the exploitation amount of petroleum are closely related to national economic development, therefore, the drilling and exploitation technology of petroleum is concerned, the petroleum exploitation firstly needs to drill a well near an oil field, during the drilling process, as a drill bit continuously deepens underground, the geological structure becomes more and more complex, at present, the biggest difficult problems encountered in the drilling industry are that the clay mineral content of a shale stratum is high, the drilling fluid used in the drilling process is in contact with the clay mineral of the shale stratum for a long time, the clay of the shale stratum can generate a serious hydration expansion phenomenon, the wall instability of a shale stratum well section is caused, further complex conditions such as collapse of the well wall and drill bit pause are caused, the cost and the period of drilling are increased, and therefore, the improvement of the inhibitability of the drilling fluid becomes a research hotspot.
The amine substance can adhere clay lamella together through the actions of electrostatic adsorption, hydrogen bond and the like, so that water molecules are difficult to permeate among the clay lamellae, and the clay lamella inhibitor has good clay hydration expansion inhibiting performance, so that the low molecular weight inhibitor which is used as a drilling fluid inhibitor for a long time and has the application number of CN201610644344.5 discloses an ultralow molecular weight intercalation inhibitor and a preparation method thereof. The Chinese patent with the application number of CN202010288432.2 discloses an environment-friendly hyperbranched polyquaternary ammonium amino acid-supported shale intercalation inhibitor, which utilizes the electropositivity of quaternary ammonium groups to generate electrostatic adsorption with negative charges carried on the surface of clay, so that electrostatic repulsion between clay sheet layers is weakened, the clay is easier to aggregate and flocculate, and a good inhibition effect is generated.
Disclosure of Invention
The invention aims to provide an amino polymer inhibitor for drilling fluid and a preparation method thereof, wherein the prepared amino polymer inhibitor has a good inhibition effect on shale mineral clay by utilizing the double synergistic inhibition effect of primary inhibitor coating inhibition and secondary inhibitor intercalation inhibition, and the problem of borehole wall instability caused by clay hydration dispersion in the drilling process is solved.
The purpose of the invention can be realized by the following technical scheme:
an amino polymer inhibitor for drilling fluid comprises the following raw materials in parts by weight: 40-80 parts of a main inhibitor and 10-25 parts of an auxiliary inhibitor;
the structural formula of the main inhibitor is shown as follows:
wherein x, y, z and m are positive integers;
the structural formula of the secondary inhibitor is shown as follows:
wherein n is a positive integer.
Further, the preparation method of the main inhibitor specifically comprises the following steps:
uniformly mixing acrylamide, acrylic acid, 2-acrylamido-2-methylpropanesulfonic acid and N- (3-aminopropyl) methacrylate hydrochloride, neutralizing by using a sodium hydroxide solution, adding an initiator solution, stirring until the system is completely dissolved, introducing nitrogen to remove oxygen, placing the mixture in a temperature environment of 50-60 ℃, stirring and reacting for 1-3 hours, removing water by using ethanol after the reaction is finished, performing suction filtration to collect a solid product, and performing vacuum drying to obtain the main inhibitor.
Further, the concentration of the sodium hydroxide solution is 0.5-1mol/L.
Further, the initiator solution is an aqueous solution of sodium bisulfite and sodium persulfate in a mass ratio of 1.
Further, the nitrogen flow rate is 0.6-0.8L/min.
According to the technical scheme, acrylamide, acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid and N- (3-aminopropyl) methacrylate hydrochloride monomers are initiated to carry out free radical copolymerization reaction under a redox initiation system consisting of sodium bisulfite and sodium persulfate, the acidity of the system is neutralized by using sodium hydroxide, and the amino polymer main inhibitor containing amide groups, sulfonic acid groups, carboxylic acid groups and active amino groups in the structure is prepared under the protection of nitrogen.
Further, the secondary inhibitor is prepared by the following steps:
s1: dissolving 3-chloropropionyl chloride and ethylene glycol in N, N-dimethylformamide, adding an alkaline catalyst, and stirring at room temperature for 4-12h to obtain a pre-reaction solution;
s2: and (3) adding diethylenetriamine into the pre-reaction liquid, continuing stirring for 2-6h, after the reaction is finished, carrying out reduced pressure distillation, carrying out suction filtration to obtain a solid sample, washing the product with hydrochloric acid with the mass fraction of 5-10% and purified water in sequence to make the pH value of the product neutral, and carrying out vacuum drying to obtain the auxiliary inhibitor.
Further, in step S1, the molar ratio of the 3-chloropropionyl chloride to the ethylene glycol is 1.2-1.5.
Further, in step S1, the basic catalyst is pyridine.
Further, in the step S2, the amount of the diethylenetriamine is 120-160% of the total amount of the 3-chloropropionyl chloride and the ethylene glycol.
According to the technical scheme, under the action of an alkaline catalyst pyridine, an acyl chloride group in a 3-chloropropionyl chloride structure and a hydroxyl group in an ethylene glycol structure are subjected to esterification condensation reaction to form a pre-reaction liquid, and then diethylenetriamine is used for further reaction with a pre-reaction product to prepare the amine-terminated polymer auxiliary inhibitor.
The preparation method of the amino polymer inhibitor for the drilling fluid comprises the following steps: and pouring the main inhibitor and the auxiliary inhibitor into a mixer, setting the stirring speed at 300-500r/min, stirring at room temperature for 4-8h, and discharging to obtain the amino polymer inhibitor.
The invention has the beneficial effects that:
the main inhibitor prepared by the invention has moderate molecular weight, the apparent viscosity of the drilling fluid can not be greatly increased, the molecular chain structure of the main inhibitor contains amino, the amino can be adsorbed on the surface of clay minerals of the shale and is embedded between clay crystal layers, longer molecular chains can fully extend in the drilling fluid, and then the clay and drill cuttings are firmly coated by proper crosslinking, adsorption and winding effects, so that water is difficult to contact with the clay and drill cuttings, thereby effectively inhibiting the hydration expansion of the clay and drill cuttings.
The molecular chain of the prepared auxiliary inhibitor contains a large amount of primary amino functional groups and secondary amino functional groups, the primary amino functional groups and the secondary amino functional groups can show strong electropositivity in a drilling fluid system, can be preferentially adsorbed in clay shale mineral clay through electrostatic action, and then are intercalated into the interlayer of the clay mineral, mineral clay lamella are firmly adsorbed together by using the electrostatic action, and moisture is prevented from entering the interlayer of the mineral clay, so that the hydration expansion phenomenon among clay crystal layers is effectively reduced, the prepared auxiliary inhibitor is excellent in high-temperature stability, flocculation and coalescence of the drilling fluid cannot be caused, in addition, the auxiliary inhibitor is good in compatibility, can form a good composite inhibitor by using a main inhibitor, is easy to degrade, has no biotoxicity, is environment-friendly, and has no pollution.
The composite amino polymer inhibitor is prepared by combining the auxiliary inhibitor and the main inhibitor, the auxiliary inhibitor is preferentially adsorbed between mineral clay layers by utilizing the chemical potential difference to generate hydrogen bonds and electrostatic intercalation, inorganic cations are replaced, dehydration between the clay layers is promoted, the clay layers are compressed, the hydration expansion phenomenon of the clay is inhibited, the mineral clay is firmly coated in the main inhibitor by properly crosslinking, adsorbing and winding the main inhibitor on the clay surface, and moisture is prevented from permeating into the clay surface or even between the clay layers, so that the composite amino polymer inhibitor has excellent inhibition performance by combining the double inhibition effects of the main inhibitor and the auxiliary inhibitor, and the hydration dispersion problem of the clay is solved.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart illustrating the preparation of an amine-based polymer inhibitor prepared in example 1 of the present invention;
FIG. 2 is an infrared characterization plot of the primary inhibitor prepared in example 1 of the present invention;
FIG. 3 is an infrared characterization plot of the secondary inhibitors prepared in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
1. Preparation of the Primary inhibitor
Mixing 10g of acrylamide, 1.5g of acrylic acid, 0.8g of 2-acrylamido-2-methylpropanesulfonic acid and 1.2g of N- (3-aminopropyl) methacrylate hydrochloride, neutralizing with a 0.5mol/L sodium hydroxide solution, adding 10mL of an aqueous solution containing 0.1g of sodium bisulfite and 0.1g of sodium persulfate, stirring until the system is completely dissolved, setting the nitrogen flow rate to be 0.6L/min, introducing nitrogen to remove oxygen, placing the mixture in a temperature environment of 60 ℃, stirring for reaction for 2 hours, removing water by using ethanol after the reaction is finished, carrying out suction filtration to collect a solid product, and carrying out vacuum drying to obtain a main inhibitor, wherein the structural formula is as follows:
wherein x, y, z and m are positive integers; the infrared characterization is carried out, and the result is shown in figure 2, wherein the length is 3200-3500 cm -1 The peak is the stretching vibration peak of carboxylic acid-OH and amide N-H, 2800-3000 cm -1 The vibration peak is the stretching vibration peak of the saturated alkyl carbon-hydrogen bond, and is 1600-1750 cm -1 A 1068cm telescopic vibration absorption peak at C = O -1 The peak is a characteristic peak of a sulfonic acid group.
2. Preparation of secondary inhibitors
S1: dissolving 5g of 3-chloropropionyl chloride and 2g of ethylene glycol in N, N-dimethylformamide, adding 6mL of pyridine, and stirring at room temperature for 9 hours to obtain a pre-reaction solution;
s2: adding 10g of diethylenetriamine into the pre-reaction liquid, continuing stirring for 6h, after the reaction is finished, removing low-boiling-point substances through reduced pressure distillation, filtering out a solid sample, washing the product with hydrochloric acid with the mass fraction of 10% and purified water in sequence until the pH value is neutral, and performing vacuum drying to obtain an auxiliary inhibitor, wherein the structural formula is as follows:
wherein n is a positive integer; the infrared characterization is carried out, and the result is shown in figure 3, wherein the length is 3200-3500 cm -1 Is positioned at the stretching vibration peak of primary amine and secondary amine, 2800-3000 cm -1 The absorption peak is the characteristic absorption peak of a saturated alkyl chain, 1724cm -1 Peak of stretching vibration at C = O, 1060cm -1 Is the stretching vibration peak of the C-O bond.
3. Preparation of amine-based polymer inhibitors
Pouring 40 parts of main inhibitor and 10 parts of auxiliary inhibitor into a mixer, setting the stirring speed at 300r/min, stirring for 4 hours at room temperature, and discharging to obtain the amino polymer inhibitor; the preparation process of the amine-based polymer inhibitor is shown in figure 1.
Example 2
Preparation of amine-based polymer inhibitors
60 parts of the main inhibitor prepared in the embodiment 1 of the invention and 20 parts of the auxiliary inhibitor prepared in the embodiment 1 of the invention are poured into a mixer, the stirring speed is set to be 400r/min, and after stirring for 6 hours at room temperature, the mixture is discharged, thus obtaining the amino polymer inhibitor.
Example 3
Preparation of amine-based polymer inhibitors
And (3) pouring 80 parts of the main inhibitor prepared in the embodiment 1 of the invention and 25 parts of the auxiliary inhibitor prepared in the embodiment 1 of the invention into a mixer, setting the stirring speed at 500r/min, stirring at room temperature for 8 hours, and discharging to obtain the amino polymer inhibitor.
Performance detection
A. With reference to ST/T5613-2016 (test method for physicochemical properties of shale), a shale dispersion experiment is carried out to evaluate the inhibition performance of the amino polymer inhibitor prepared in the embodiments 1-3 of the invention;
a. the amine-based polymer inhibitors prepared in inventive examples 1-3 were subjected to a linear expansion experiment: weighing 5g of bentonite, pouring the bentonite into a sleeve, compacting the bentonite for 5min under the pressure of 10MPa, filling the compacted bentonite with a layer of filter paper, embedding the sleeve into a dilatometer, adding purified water, the amine-based polymer inhibitor prepared in examples 1-3 and a commercially available FA367 inhibitor respectively, recording the swelling amount of the bentonite after 1h and 16h, calculating the linear swelling rate, and evaluating the inhibition performance of the inhibitor, wherein generally, the higher the linear swelling rate is, the worse the inhibition performance is, and vice versa, wherein the FA367 inhibitor is purchased from American landscape chemical industries, inc. of Yang, and the test results are shown in the following table:
as can be seen from the above table, when the bentonite is treated with purified water, the linear expansion rate of the bentonite is as high as 43.60%, and when the inhibitor prepared in examples 1-3 of the present invention is used, the linear expansion rate of the bentonite is reduced to 8.69% at the lowest, which effectively reduces the linear expansion rate of the bentonite, and the inhibition performance is obviously better than that of the commercial inhibitor.
b. In the rock debris recovery experiments performed on the inhibitors of examples 1 to 3 of the present invention and on the market, generally, the higher the rock debris recovery, the better the inhibition performance, and vice versa, the worse the sandstone was used as the rock sample, and the test results are shown in the following table:
as can be seen from the above table, at the hot rolling temperature of 150 ℃, the recovery rate of the rock debris of the purified water is only 2.52%, while the inhibitors prepared in examples 1 to 3 of the present invention all have higher recovery rate of the rock debris and are significantly higher than the commercial inhibitors, so the inhibitors prepared in examples 1 to 3 of the present invention have good inhibition effect.
B. Compatibility test: pouring 100g of bentonite and 2L of water into a stirrer, stirring for 20min, sequentially adding 10g of PMHC-I tackifier, 10g of XY-27 viscosity reducer, 5g of SPNH fluid loss additive, 10g of RT-001 lubricant and 1kg of barite into the stirrer under the condition of continuous stirring to prepare drilling fluid, mixing two parts of drilling fluid with equal amount with 2% of inhibitor prepared in the embodiments 1 to 3 of the invention, and testing the rheological property of the drilling fluid after hot rolling at room temperature and 120 ℃ respectively, wherein the test results are shown in the following table:
as can be seen from the above table, after the inhibitors prepared in examples 1 to 3 of the present invention are added, the change values of the apparent viscosity, the molding viscosity and the dynamic shear force of the drilling fluid are small, which indicates that the prepared inhibitors have good compatibility, and after the drilling fluid is subjected to hot rolling treatment at 120 ℃, the change of the fluidity of the drilling fluid is not large, which indicates that the prepared inhibitors have good temperature resistance.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (10)
1. The amino polymer inhibitor for the drilling fluid is characterized by comprising the following raw materials in parts by weight: 40-80 parts of a main inhibitor and 10-25 parts of an auxiliary inhibitor;
the structural formula of the main inhibitor is shown as follows:
the structural formula of the secondary inhibitor is shown as follows:
2. The amine-based polymer inhibitor for drilling fluid as claimed in claim 1, wherein the preparation method of the main inhibitor comprises the following specific steps:
uniformly mixing acrylamide, acrylic acid, 2-acrylamido-2-methylpropanesulfonic acid and N- (3-aminopropyl) methacrylate hydrochloride, neutralizing by using a sodium hydroxide solution, adding an initiator solution, stirring until the system is completely dissolved, introducing nitrogen to remove oxygen, placing the mixture in a temperature environment of 50-60 ℃, stirring and reacting for 1-3 hours, removing water by using ethanol after the reaction is finished, carrying out suction filtration to collect a solid product, and carrying out vacuum drying to obtain the main inhibitor.
3. The amine-based polymer inhibitor for drilling fluid as claimed in claim 2, wherein the concentration of the sodium hydroxide solution is 0.5-1mol/L.
4. The amine-based polymer inhibitor for drilling fluid according to claim 2, wherein the initiator solution is an aqueous solution of sodium bisulfite and sodium persulfate in a mass ratio of 1.
5. The amine-based polymer inhibitor for drilling fluid as claimed in claim 2, wherein the nitrogen flow rate is 0.6-0.8L/min.
6. The amine-based polymer inhibitor for drilling fluids according to claim 1, wherein the secondary inhibitor is prepared by the following steps:
s1: dissolving 3-chloropropionyl chloride and ethylene glycol in N, N-dimethylformamide, adding an alkaline catalyst, and stirring at room temperature for 4-12h to obtain a pre-reaction solution;
s2: and (3) adding diethylenetriamine into the pre-reaction liquid, continuing stirring for 2-6h, after the reaction is finished, carrying out reduced pressure distillation, carrying out suction filtration to obtain a solid sample, washing the product with hydrochloric acid with the mass fraction of 5-10% and purified water in sequence to make the pH value of the product neutral, and carrying out vacuum drying to obtain the auxiliary inhibitor.
7. The amine-based polymer inhibitor for drilling fluid according to claim 6, wherein in the step S1, the molar ratio of the 3-chloropropionyl chloride to the ethylene glycol is 1.2-1.5.
8. The amine-based polymer inhibitor for drilling fluid as claimed in claim 6, wherein in step S1, the basic catalyst is pyridine.
9. The amine-based polymer inhibitor for drilling fluid according to claim 6, wherein in the step S2, the addition amount of the diethylenetriamine is 120-160% of the total amount of the 3-chloropropionyl chloride and the ethylene glycol.
10. The preparation method of the amine-based polymer inhibitor for drilling fluid according to claim 1, wherein the preparation method comprises the following specific steps: and pouring the main inhibitor and the auxiliary inhibitor into a mixer, setting the stirring speed at 300-500r/min, stirring at room temperature for 4-8h, and discharging to obtain the amino polymer inhibitor.
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