CN114989423A - Sedimentation stabilizing composition, sedimentation stabilizing agent and preparation method and application thereof - Google Patents
Sedimentation stabilizing composition, sedimentation stabilizing agent and preparation method and application thereof Download PDFInfo
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- CN114989423A CN114989423A CN202210645793.7A CN202210645793A CN114989423A CN 114989423 A CN114989423 A CN 114989423A CN 202210645793 A CN202210645793 A CN 202210645793A CN 114989423 A CN114989423 A CN 114989423A
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
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Abstract
The invention provides a settlement stabilizing composition, a settlement stabilizing agent, a preparation method and application thereof. The sedimentation stabilizing composition comprises: 260-320 parts of oleic acid and/or tall oil acid, 90-110 parts of organic amine, 70-100 parts of 3,4, 5-trihydroxybenzoic acid, 150-180 parts of humic acid and 50-70 parts of citric acid and/or maleic anhydride. The sedimentation stabilizing agent is prepared by adopting the sedimentation stabilizing composition to carry out dehydration condensation reaction. The invention also provides application of the settling stabilizer in a gas-to-oil synthetic base drilling fluid system. The settlement stabilizing composition has the advantages of simple formula, wide sources of monomer raw materials and relatively low production cost, and the settlement stabilizing agent prepared from the settlement stabilizing composition has excellent high-temperature settlement stabilizing performance and high-temperature rheological stabilizing performance of barite.
Description
Technical Field
The invention relates to a sedimentation stabilizing composition, a sedimentation stabilizing agent, a preparation method and application thereof, and belongs to the technical field of drilling.
Background
In recent years, with the increasing demand of energy, oil exploration and development gradually drill towards deep parts and complex stratums, the number of complex wells such as deep drilling wells, ultra-deep wells, large-inclination directional wells, large-displacement horizontal wells and the like is increased, more unconventional oil and gas resources are developed, and the demand of oil bases, particularly environment-friendly gas-to-oil synthetic base drilling fluids is increased gradually. The gas-to-oil synthetic-based drilling fluid system is a novel drilling fluid system with environmental protection characteristics, has the characteristics of high temperature resistance, salt and calcium corrosion resistance, contribution to well wall stability, good lubricity, small damage to an oil-gas layer and the like of the oil-based drilling fluid, and also has the advantages of low kinematic viscosity, high mechanical drilling speed, environmental friendliness and the like.
The gas-to-oil synthetic-based drilling fluid system has the advantages that the adopted gas-to-oil is synthesized by catalytic hydrogenation of natural gas, does not contain harmful substances such as aromatic hydrocarbon, sulfur, amine and the like, is easy to biodegrade, is more environment-friendly, and has low kinematic viscosity of 2.6 (mm) 2 40 ℃ (5# white oil and 0# diesel oil have kinematic viscosities of 3.86 and 3.4 (mm) respectively 2 40/s)), which is advantageous for reducing the Equivalent Circulating Density (ECD) of the drilling fluid and increasing the solid content. However, because the gas-to-oil kinematic viscosity is low and aromatic hydrocarbons are not contained, the efficiency of the organic soil with good colloid rate and viscosity-increasing and shear-improving effects in the oil-based drilling fluid system is reduced or lost in the gas-to-oil synthetic-based drilling fluid system, so that the problems of poor high-temperature rheological stability, easy settlement of barite and the like of the gas-to-oil synthetic-based drilling fluid system are caused.
Therefore, the development of a settling stabilizer suitable for a gas-to-oil synthetic base drilling fluid system becomes one of the problems to be solved in the field.
Disclosure of Invention
In order to solve the above technical problems, the present invention aims to provide a sedimentation stabilizing composition. The invention also aims to provide a sedimentation stabilizing agent, a preparation method and an application thereof, wherein the sedimentation stabilizing agent is prepared by adopting the sedimentation stabilizing composition. The settling stabilizer provided by the invention is suitable for being applied to a gas-to-oil synthetic base drilling fluid system, and has excellent high-temperature rheological stability and barite settling stability.
In order to achieve the above object, the present invention provides, in a first aspect, a sedimentation stabilizing composition comprising, in parts by weight: 260-320 parts of oleic acid and/or tall oil acid, 90-110 parts of organic amine, 70-100 parts of 3,4, 5-trihydroxybenzoic acid, 150-180 parts of humic acid and 50-70 parts of citric acid and/or maleic anhydride.
According to an embodiment of the present invention, preferably, the sedimentation stabilizing composition further comprises 150-200 parts by weight of a solvent. More preferably, the solvent comprises white oil and/or mineral spirits D80. More preferably, the white oil comprises number 3 white oil. The present invention preferably employs mineral spirits D80 and/or white oil No. 3, which have low viscosity and good solubility and are suitable for use in the sedimentation stabilizing compositions of the present invention.
In the above-mentioned sedimentation stabilizing composition, preferably, the organic amine includes one or a combination of several of tetraethylenepentamine, diethylenetriamine, diethanolamine, and the like. More preferably, the organic amine is tetraethylenepentamine. The molecular chain of the tetraethylenepentamine has more amino functional groups, and the macromolecular polycondensate formed by dehydrating and condensing the tetraethylenepentamine and other components in the sedimentation stabilizing composition has more hydrophilic groups.
In a second aspect, the present invention provides a sedimentation stabilizer prepared by a dehydration condensation reaction using the above sedimentation stabilizing composition.
According to a particular embodiment of the present invention, preferably, the sedimentation stabilizer is prepared by at least the following steps:
step S1, according to the weight parts, carrying out a first dehydration condensation reaction on the oleic acid and/or tall oil acid and the organic amine to obtain a first post-reaction system;
step S2, carrying out a second dehydration condensation reaction on the first reacted system and the 3,4, 5-trihydroxybenzoic acid to obtain a second reacted system;
step S3, carrying out a third dehydration condensation reaction on the second reacted system and the humic acid to obtain a third reacted system;
and step S4, carrying out fourth dehydration condensation reaction on the third reacted system and the citric acid and/or the maleic anhydride to obtain a fourth reacted system, namely the sedimentation stabilizer.
More preferably, the preparation step of the sedimentation stabilizer further comprises: and step S5, cooling the system after the fourth reaction to a certain temperature, and mixing the system with the solvent according to the parts by weight to obtain the settling stabilizer.
The sedimentation stabilizing agent obtained after the sedimentation stabilizing composition of the invention is subjected to the steps S1-S4 has higher viscosity due to the larger relative molecular weight (the molecular weight is estimated to be 3000-5000g/mol), and is solid paste at normal temperature. In order to facilitate the on-site pouring and use and reduce the product cost, solvent oil D80 and/or No. 3 white oil are preferably used as solvents, and the solvent oil has the advantages of applicable viscosity, low price and safe use.
In the above-mentioned sedimentation stabilizer, it is preferable that the temperature of the first dehydrating condensation reaction in the step S1 is 150-180 ℃ for 3-5 h.
In the above-mentioned sedimentation stabilizer, it is preferable that the temperature of the second dehydration condensation reaction in step S2 is 150-180 ℃ for 2-4 h.
In the above-mentioned sedimentation stabilizer, it is preferable that the temperature of the third dehydration condensation reaction in the step S3 is 150-180 ℃ for 2-4 h.
In the above-mentioned sedimentation stabilizer, it is preferable that the temperature of the fourth dehydration condensation reaction in the step S4 is 150-180 ℃ for 2-4 h.
In the above-mentioned sedimentation stabilizer, preferably, in step S5, the system after the fourth reaction is cooled to 120-.
In the above-mentioned sedimentation stabilizer, preferably, the first dehydration condensation reaction, the second dehydration condensation reaction, the third dehydration condensation reaction and the fourth dehydration condensation reaction are all performed under stirring, and the rotation speed of the stirring is 180-250 rpm respectively.
The present invention creatively uses the five monomers having amino group and carboxyl group, and forms a high-molecular polycondensate having a crosslinked structure by dehydrating and condensing them. The crosslinking density of the polymer polycondensate formed by the specific weight parts of the monomers is beneficial to fully inhibiting the sliding among molecular chains of the polymer polycondensate and increasing the hardness and modulus of the polymer polycondensate, so that the polymer polycondensate has higher stability. When the settling stabilizer formed by the high-molecular polycondensate is applied to the gas-to-oil synthetic base drilling fluid, on one hand, hydrophilic groups such as amino groups and imino groups in the main chain segment of the settling stabilizer polycondensate act on the surface of the barite, and unsaturated hydrocarbon lipophilic branched chain segments formed after condensation of oleic acid and/or tall oil acid are dissolved and dispersed in the gas-to-oil base fluid, so that the effect of suspending the barite is achieved, the settling of the barite can be effectively prevented, and the settling stability of the barite of a drilling fluid system is improved. On the other hand, the stability of the high-molecular polycondensate is beneficial to reducing the probability of poor rheological property of a drilling fluid system caused by decomposition of the high-molecular polycondensate in the use process of the high-temperature drilling fluid. Particularly for a high-temperature-resistant gas-to-oil synthetic-based drilling fluid system with higher requirement on the environmental protection property of a treating agent, the sedimentation stabilizer is beneficial to improving the high-temperature rheological property and the barite sedimentation stability of the gas-to-oil synthetic-based drilling fluid system, so that the problems of poor high-temperature rheological property, barite sedimentation and the like of the high-density gas-to-oil synthetic-based drilling fluid system are solved. Meanwhile, the settlement stabilizer disclosed by the invention is simple in formula, cheap and easily available in raw materials, and the production cost is reduced.
The third aspect of the present invention provides a preparation method of the above sedimentation stabilizer, which comprises the following steps:
step S1, according to the weight parts, carrying out a first dehydration condensation reaction on the oleic acid and/or tall oil acid and the organic amine to obtain a first post-reaction system;
step S2, carrying out a second dehydration condensation reaction on the first reacted system and the 3,4, 5-trihydroxybenzoic acid to obtain a second reacted system;
step S3, carrying out a third dehydration condensation reaction on the second reacted system and the humic acid to obtain a third reacted system;
and step S4, carrying out a fourth dehydration condensation reaction on the third reacted system and the citric acid and/or the maleic anhydride to obtain a fourth reacted system, namely the sedimentation stabilizer.
According to a specific embodiment of the present invention, preferably, the above preparation method further comprises: and step S5, cooling the system after the fourth reaction to a certain temperature, and mixing the system with the solvent according to the parts by weight to obtain the settling stabilizer.
In the above preparation method, preferably, the temperature of the first dehydration condensation reaction in step S1 is 150 ℃ and 180 ℃ for 3-5 h. The reaction temperature is preferably in the above range in order to achieve both the efficiency of the first dehydration condensation reaction and the reduction of the probability of occurrence of side reactions due to an excessively high temperature. The time of the first dehydrating condensation reaction is preferably 3 to 5 hours, which helps to control the first dehydrating condensation reaction to be carried out to such an extent that moisture is not generated, i.e., the reaction is substantially completed.
In the above preparation method, preferably, the temperature of the second dehydration condensation reaction in step S2 is 150-180 ℃ for 2-4 h.
In the above preparation method, preferably, the temperature of the third dehydration condensation reaction in step S3 is 150-180 ℃ for 2-4 h.
In the above preparation method, preferably, the temperature of the fourth dehydration condensation reaction in step S4 is 150-180 ℃ for 2-4 h.
In the preparation method, preferably, in step S5, the temperature of the system after the fourth reaction is reduced to 120-140 ℃, and then the system is mixed with the solvent. In order to prepare the settling stabilizer with proper viscosity and concentration and convenient field use, the settling stabilizer is dissolved and diluted by a solvent (preferably solvent oil D80 and/or white oil No. 3), wherein the solvent is also important for the dilution temperature of the settling stabilizer, materials can boil and overflow during the dilution process at too high temperature, and the materials are solidified at too low temperature and cannot be dissolved and diluted. The solvent-dissolving dilution temperature in the above step S5 is preferably 120-140 ℃.
In the above preparation method, preferably, the first dehydrating condensation reaction, the second dehydrating condensation reaction, the third dehydrating condensation reaction and the fourth dehydrating condensation reaction are all performed under stirring, and the rotation speed of the stirring is 180 revolutions per minute and 250 revolutions per minute respectively.
In the above production method of the present invention, first, oleic acid and/or tall oil acid, and an organic amine (preferably tetraethylenepentamine) are subjected to first dehydrating condensation, and then, to second dehydrating condensation with 3,4, 5-trihydroxybenzoic acid, and then, to third dehydrating condensation with humic acid, and then, to fourth dehydrating condensation with citric acid and/or maleic anhydride. The condensation sequence of the monomers determines the cross-linking structure of the formed high-molecular polycondensate, and the specific monomers and the condensation sequence thereof adopted by the invention are more favorable for ensuring that the prepared settling stabilizer has high-temperature rheological stability and barite settling stability. Meanwhile, the preparation method of the sedimentation stabilizer has the advantages of wide sources of raw materials for preparing the monomers, simple preparation method and the like.
The invention provides an application of the settling stabilizer in a gas-to-oil synthetic base drilling fluid system.
In the application, the use temperature of the gas-to-oil synthesis-based drilling fluid system is preferably below 200 ℃, and more preferably 120-200 ℃.
In the application, the oil-water volume ratio of the gas-to-oil synthetic-based drilling fluid system is preferably 70: 30-90: 10.
In the application, the density of the gas-to-oil synthetic-based drilling fluid system is preferably 1.8-2.2 g/cm 3 。
The sedimentation stabilizer provided by the invention has excellent high-temperature rheological stability and barite sedimentation prevention performance, has important significance in being applied to a high-temperature resistant drilling fluid system, and particularly has high-temperature stability which can reduce the occurrence probability of poor performance of the drilling fluid system caused by decomposition of the sedimentation stabilizer in the high-temperature use process. In consideration of the economic benefit of the application of the settling stabilizer, the invention applies the settling stabilizer to a gas-to-oil synthetic-based drilling fluid system with higher requirement on environmental protection, and in order to further improve the use efficiency of the settling stabilizer in the gas-to-oil synthetic-based drilling fluid system, the temperature, the density and the oil-water ratio of the gas-to-oil synthetic-based drilling fluid system are preferably within the ranges. Wherein the gas-to-oil synthetic base drilling fluid system with the temperature of 200 ℃ also further illustrates the excellent performance of the settling stabilizer.
The five monomers are adopted to form the high-molecular polycondensate containing a cross-linking structure through dehydration condensation, and the cross-linking density of the high-molecular polycondensate formed by the monomers is beneficial to fully inhibiting the sliding among the molecular chains of the high-molecular polycondensate and increasing the hardness and the modulus of the high-molecular polycondensate, so that the high-molecular polycondensate has higher stability. In addition, the long linear chain alkyl in the high-molecular polycondensation product can form a three-dimensional network structure through association with synthetic oil in the gas-to-oil synthetic base drilling fluid, so that the oil-soluble suspension performance of the settling stabilizer is enhanced; and the polar groups such as amino, imino and amido can interact with the surface of the barite through electrostatic attraction or hydrogen bonds, so that the settling stability and rheological property of the barite in a synthetic base drilling fluid system are enhanced. The polymer polycondensate is used as the sedimentation stabilizer of the gas-to-oil synthetic-based drilling fluid system, and the suspension property and the rheological property of the barite of the gas-to-oil synthetic-based drilling fluid system are improved through the two effects, so that the sedimentation stability of the barite is enhanced, and the problems of poor high-temperature rheological property, barite sedimentation and the like of the gas-to-oil synthetic-based drilling fluid system due to the fact that the viscous shear force of organic soil in gas-to-oil is reduced in the process of drilling a large-inclination directional well and a large-displacement horizontal well are solved.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
This example provides a sedimentation stabilizer prepared by the following steps:
sequentially adding 286 parts of oleic acid and 95 parts of tetraethylenepentamine into a reactor by weight, heating to 165 ℃ under continuous stirring (the stirring speed is 200 revolutions per minute, and the following dehydration condensation reactions are all carried out at the stirring speed), and carrying out dehydration condensation reaction for 3 hours to obtain a first post-reaction system; adding 85 parts of 3,4, 5-trihydroxybenzoic acid, and carrying out a second dehydration condensation reaction at 165 ℃ for 2 hours to obtain a second reaction system; adding 155 parts of humic acid, and carrying out a third dehydration condensation reaction at 165 ℃ for 2h to obtain a third post-reaction system; and adding 64 parts of citric acid, and carrying out a fourth dehydration condensation reaction at 165 ℃ for 2h to obtain a fourth reaction system. And after the reaction is finished, cooling to 120 ℃, slowly adding 170 parts of No. 3 white oil, and dissolving and diluting the system after the fourth reaction. And cooling to 80 ℃, and discharging to obtain the finished product of the sedimentation stabilizer, which is marked as sedimentation stabilizer A.
Example 2
This example provides a sedimentation stabilizer prepared by the following steps:
sequentially adding 300 parts by weight of oleic acid and 97 parts by weight of tetraethylenepentamine into a reactor, heating to 165 ℃ under continuous stirring (the stirring speed is 200 revolutions per minute, and the following dehydration condensation reactions are all carried out at the stirring speed), and carrying out dehydration condensation reaction for 3 hours to obtain a first post-reaction system; adding 75 parts of 3,4, 5-trihydroxybenzoic acid, and carrying out a second dehydration condensation reaction at 165 ℃ for 2h to obtain a second reaction system; adding 180 parts of humic acid, and carrying out a third dehydration condensation reaction at 165 ℃ for 2h to obtain a third post-reaction system; and adding 70 parts of citric acid, and carrying out a fourth dehydration condensation reaction for 2 hours at 165 ℃ to obtain a fourth reaction system. And after the reaction is finished, cooling to 120 ℃, slowly adding 180 parts of No. 3 white oil, and dissolving and diluting the system after the fourth reaction. And cooling to 80 ℃, and discharging to obtain a finished sedimentation stabilizer product marked as sedimentation stabilizer B.
Example 3
This example provides a sedimentation stabilizer prepared by the following steps:
adding 260 parts by weight of oleic acid and 90 parts by weight of tetraethylenepentamine into a reactor in sequence, heating to 165 ℃ under continuous stirring (the stirring speed is 200 revolutions per minute, and the following dehydration condensation reactions are all carried out at the stirring speed), and carrying out dehydration condensation reaction for 3 hours to obtain a first post-reaction system; adding 92 parts of 3,4, 5-trihydroxybenzoic acid, and carrying out a second dehydration condensation reaction at 165 ℃ for 2 hours to obtain a second reaction system; adding 150 parts of humic acid, and carrying out a third dehydration condensation reaction at 165 ℃ for 2h to obtain a third post-reaction system; then 58 parts of citric acid is added, and the fourth dehydration condensation reaction is carried out for 2 hours at 165 ℃ to obtain a fourth reaction system. And after the reaction is finished, cooling to 120 ℃, slowly adding 160 parts of No. 3 white oil, and dissolving and diluting the system after the fourth reaction. And cooling to 80 ℃, and discharging to obtain a finished sedimentation stabilizer product marked as sedimentation stabilizer C.
Example 4
This example provides a sedimentation stabilizer prepared by the following steps:
adding 320 parts by weight of oleic acid and 100 parts by weight of tetraethylenepentamine into a reactor in sequence, heating to 165 ℃ under continuous stirring (the stirring speed is 200 revolutions per minute, and the following dehydration condensation reactions are all carried out at the stirring speed), and carrying out dehydration condensation reaction for 3 hours to obtain a first post-reaction system; adding 100 parts of 3,4, 5-trihydroxybenzoic acid, and carrying out a second dehydration condensation reaction at 165 ℃ for 2h to obtain a second reaction system; adding 150 parts of humic acid, and carrying out a third dehydration condensation reaction at 165 ℃ for 2h to obtain a third post-reaction system; then 60 parts of maleic anhydride is added, and the fourth dehydration condensation reaction is carried out for 2 hours at 165 ℃ to obtain a fourth reaction system. And after the reaction is finished, cooling to 120 ℃, slowly adding 180 parts of No. 3 white oil, and dissolving and diluting the system after the fourth reaction. And cooling to 80 ℃, and discharging to obtain a finished product of the sedimentation stabilizer, which is marked as sedimentation stabilizer D.
Comparative example 1
The present comparative example provides a sedimentation stabilizer, which is prepared by the following steps:
sequentially adding 400 parts by weight of oleic acid and 95 parts by weight of tetraethylenepentamine into a reactor, heating to 165 ℃ under continuous stirring (the stirring speed is 200 revolutions per minute, and the following dehydration condensation reactions are all carried out at the stirring speed), and carrying out dehydration condensation reaction for 3 hours to obtain a first post-reaction system; adding 40 parts of 3,4, 5-trihydroxybenzoic acid, and carrying out a second dehydration condensation reaction at 165 ℃ for 2h to obtain a second reaction system; adding 220 parts of humic acid, and carrying out a third dehydration condensation reaction at 165 ℃ for 2h to obtain a third post-reaction system; and adding 70 parts of citric acid, and carrying out a fourth dehydration condensation reaction for 2 hours at 165 ℃ to obtain a fourth reaction system. And after the reaction is finished, cooling to 120 ℃, slowly adding 200 parts of No. 3 white oil, and dissolving and diluting the system after the fourth reaction. And (4) cooling to 80 ℃, discharging to obtain a finished product of the sedimentation stabilizer of the comparative example, which is marked as sedimentation stabilizer E.
Comparative example 2
The present comparative example provides a sedimentation stabilizer, which is prepared by the following steps:
sequentially adding 200 parts by weight of oleic acid and 80 parts by weight of tetraethylenepentamine into a reactor, heating to 165 ℃ under continuous stirring (the stirring speed is 200 revolutions per minute, and the following dehydration condensation reactions are all carried out at the stirring speed), and carrying out dehydration condensation reaction for 3 hours to obtain a first post-reaction system; adding 50 parts of 3,4, 5-trihydroxybenzoic acid, and carrying out a second dehydration condensation reaction at 165 ℃ for 2h to obtain a second reaction system; adding 250 parts of humic acid, and carrying out a third dehydration condensation reaction at 165 ℃ for 2h to obtain a third post-reaction system; and adding 70 parts of citric acid, and carrying out a fourth dehydration condensation reaction for 2 hours at 165 ℃ to obtain a fourth reaction system. And after the reaction is finished, cooling to 120 ℃, slowly adding 160 parts of No. 3 white oil, and dissolving and diluting the system after the fourth reaction. And cooling to 80 ℃, discharging to obtain a finished product of the sedimentation stabilizer of the comparative example, which is marked as sedimentation stabilizer F.
Comparative example 3
The present comparative example provides a sedimentation stabilizer, which is prepared by the following steps:
adding 450 parts by weight of oleic acid and 100 parts by weight of tetraethylenepentamine into a reactor in sequence, heating to 165 ℃ under continuous stirring (the stirring speed is 200 revolutions per minute, and the following dehydration condensation reactions are all carried out at the stirring speed), and carrying out dehydration condensation reaction for 3 hours to obtain a first post-reaction system; adding 120 parts of 3,4, 5-trihydroxybenzoic acid, and carrying out a second dehydration condensation reaction at 165 ℃ for 2 hours to obtain a second reaction system; adding 90 parts of humic acid, and carrying out a third dehydration condensation reaction at 165 ℃ for 2h to obtain a third post-reaction system; and then 50 parts of citric acid is added, and the fourth dehydration condensation reaction is carried out for 2 hours at 165 ℃ to obtain a fourth reaction system. And after the reaction is finished, cooling to 120 ℃, slowly adding 200 parts of No. 3 white oil, and dissolving and diluting the system after the fourth reaction. And cooling to 80 ℃, discharging to obtain a finished product of the sedimentation stabilizer of the comparative example, which is marked as sedimentation stabilizer G.
Comparative example 4
The present comparative example provides a sedimentation stabilizer, which is prepared by the following steps:
adding 290 parts by weight of oleic acid and 90 parts by weight of tetraethylenepentamine into a reactor in sequence, heating to 165 ℃ under continuous stirring (the stirring speed is 200 revolutions per minute, and the following dehydration condensation reactions are all carried out at the stirring speed), and carrying out dehydration condensation reaction for 3 hours to obtain a first post-reaction system; adding 80 parts of 3,4, 5-trihydroxybenzoic acid, and carrying out a second dehydration condensation reaction at 165 ℃ for 2 hours to obtain a second reaction system; and adding 64 parts of citric acid, and carrying out a third dehydration condensation reaction at 165 ℃ for 2h to obtain a third post-reaction system. And after the reaction is finished, cooling to 120 ℃, slowly adding 130 parts of No. 3 white oil, and dissolving and diluting the system after the third reaction. And cooling to 80 ℃, discharging to obtain a finished product of the sedimentation stabilizer of the comparative example, and marking as the sedimentation stabilizer H.
Comparative example 5
The present comparative example provides a sedimentation stabilizer, which is prepared by the following steps:
sequentially adding 300 parts by weight of oleic acid and 100 parts by weight of tetraethylenepentamine into a reactor, heating to 165 ℃ under continuous stirring (the stirring speed is 200 revolutions per minute, and the following dehydration condensation reactions are all carried out at the stirring speed), and carrying out dehydration condensation reaction for 3 hours to obtain a first post-reaction system; adding 180 parts of humic acid, and carrying out a second dehydration condensation reaction at 165 ℃ for 2h to obtain a second reaction system; adding 50 parts of citric acid, and carrying out a third dehydration condensation reaction at 165 ℃ for 2h to obtain a third reaction system. And after the reaction is finished, cooling to 120 ℃, slowly adding 170 parts of No. 3 white oil, and dissolving and diluting the system after the third reaction. And cooling to 80 ℃, discharging to obtain a finished product of the sedimentation stabilizer of the comparative example, which is marked as sedimentation stabilizer I.
Comparative example 6
The present comparative example provides a sedimentation stabilizer, which is prepared by the following steps: sequentially adding 250 parts by weight of oleic acid and 80 parts by weight of tetraethylenepentamine into a reactor, heating to 165 ℃ under continuous stirring (the stirring speed is 200 revolutions per minute, and the following dehydration condensation reactions are all carried out at the stirring speed), and carrying out dehydration condensation reaction for 3 hours to obtain a first reaction system; adding 120 parts of humic acid, and carrying out a second dehydration condensation reaction at 165 ℃ for 2h to obtain a second reaction system; adding 40 parts of maleic anhydride, and carrying out a third dehydration condensation reaction at 165 ℃ for 2h to obtain a third post-reaction system. And after the reaction is finished, cooling to 120 ℃, slowly adding 170 parts of No. 3 white oil, and dissolving and diluting the system after the third reaction. And cooling to 80 ℃, discharging to obtain a finished product of the sedimentation stabilizer of the comparative example, which is marked as sedimentation stabilizer J.
The performance of the sedimentation stabilizers a to J will be tested in combination with specific experimental conditions.
The basic formula of the drilling fluid is as follows:
the basic formula is as follows: 80 parts of gas-to-liquid 185V +20 parts of CaCl 2 Aqueous solution (mass concentration is 20%) +3 parts of main emulsionEMUL-2W +2 parts of auxiliary emulsifier COEM-2S +2 parts of organic soil HF-120B +4 parts of fluid loss additive DRF-2L +2 parts of calcium oxide +300 parts of barite.
The test formulation: 80 parts of gas-to-liquid 185V +20 parts of CaCl 2 An aqueous solution (the mass concentration is 20%) +3 parts of a primary emulsifier EMUL-2W +2 parts of a secondary emulsifier COEM-2S +2 parts of an organic soil HF-120B +4 parts of a fluid loss additive DRF-2L +2 parts of calcium oxide +2 parts of a sedimentation stabilizer +300 parts of barite.
The settlement stabilizers A to J are respectively combined with a basic formula to prepare corresponding test formulas, the performance of each drilling fluid is measured according to the national standard number GB/T16783.2-2012, the settlement stability coefficient of barite is calculated according to the formula (1), and the test results are listed in Table 1.
Disclosure (1): SF ═ rho bottom/(rho bottom + rho top)
In the formula:
rhotop-density of the upper part of the drilling fluid column (lower layer of free liquid)
Rho bottom-density of drilling fluid column bottoms
TABLE 1 gas to oil synthetic base drilling fluid Performance results
As can be seen from the experimental results of table 1: the sedimentation stabilizers A to D for the gas-to-oil synthetic base drilling fluid prepared in the embodiments 1 to 4 have good high-temperature barite sedimentation stability within the temperature range of 200 ℃, have small change of the upper and lower density difference of a high-temperature aging gas-to-oil synthetic base drilling fluid system, have good high-temperature rheological stability, and are beneficial to improving the electrical stability of the synthetic base drilling fluid system. The barite stability of the gas-to-oil synthetic base drilling fluid system prepared by the settling stabilizers E to J of the comparative example is lower than that of the drilling fluid system prepared by the settling stabilizers A to D of the examples 1 to 4.
From the above description, it can be seen that the embodiments of the present invention achieve the following technical effects:
the invention adopts the five monomers to form the high-molecular polycondensate containing a cross-linking structure through dehydration condensation, and the cross-linking density of the high-molecular polycondensate formed by the specific weight parts of the monomers is favorable for fully inhibiting the sliding among molecular chains of the high-molecular polycondensate and increasing the hardness and the modulus of the high-molecular polycondensate, so that the high-molecular polycondensate has higher stability. In addition, the long linear chain alkyl in the high-molecular polycondensation product can form a three-dimensional network structure through association with synthetic oil in the gas-to-oil synthetic base drilling fluid, so that the oil-soluble suspension performance of the settling stabilizer is enhanced; and the polar groups such as amino, imino and amido can interact with the surface of the barite through electrostatic attraction or hydrogen bonds, so that the settling stability and rheological property of the barite in a synthetic base drilling fluid system are enhanced. The high-molecular polycondensate is used as the sedimentation stabilizer of the gas-to-oil synthetic-based drilling fluid system, and the barite suspension property and the rheological property of the gas-to-oil synthetic-based drilling fluid system are improved through the two functions, so that the barite sedimentation stability of the gas-to-oil synthetic-based drilling fluid system is enhanced.
Therefore, the settlement stabilizing composition has the advantages of simple formula, wide monomer raw material source and relatively low production cost, and the settlement stabilizing agent prepared from the settlement stabilizing composition has excellent high-temperature settlement stabilizing performance and high-temperature rheological stabilizing performance of barite.
Claims (14)
1. A sedimentation stabilizing composition comprising, in parts by weight: 260-320 parts of oleic acid and/or tall oil acid, 90-110 parts of organic amine, 70-100 parts of 3,4, 5-trihydroxybenzoic acid, 150-180 parts of humic acid and 50-70 parts of citric acid and/or maleic anhydride.
2. The sedimentation stable composition as claimed in claim 1, further comprising 150 and 200 parts by weight of a solvent; preferably, the solvent comprises white oil and/or mineral spirits D80; more preferably, the white oil comprises number 3 white oil.
3. The sedimentation stable composition of claim 1, wherein the organic amine comprises one or a combination of tetraethylenepentamine, diethylenetriamine, and diethanolamine; preferably, the organic amine is tetraethylenepentamine.
4. A sedimentation stabilizer produced by a dehydration condensation reaction using the sedimentation stabilizing composition according to any one of claims 1 to 3.
5. The sedimentation stabilizer according to claim 4, which is prepared by at least the following steps:
step S1, according to the weight parts, carrying out a first dehydration condensation reaction on the oleic acid and/or tall oil acid and the organic amine to obtain a first post-reaction system;
step S2, carrying out a second dehydration condensation reaction on the first reacted system and the 3,4, 5-trihydroxybenzoic acid to obtain a second reacted system;
step S3, carrying out a third dehydration condensation reaction on the second reacted system and the humic acid to obtain a third reacted system;
and step S4, carrying out fourth dehydration condensation reaction on the third reacted system and the citric acid and/or the maleic anhydride to obtain a fourth reacted system, namely the sedimentation stabilizer.
6. The sedimentation stabilizer according to claim 5, wherein the preparation step of the sedimentation stabilizer further comprises: and step S5, cooling the system after the fourth reaction to a certain temperature, and mixing the system with the solvent according to the parts by weight to obtain the settling stabilizer.
7. A method of preparing the sedimentation stabilizer of any one of claims 4 to 6, comprising the steps of:
step S1, according to the weight parts, carrying out a first dehydration condensation reaction on the oleic acid and/or tall oil acid and the organic amine to obtain a first post-reaction system;
step S2, carrying out a second dehydration condensation reaction on the first reacted system and the 3,4, 5-trihydroxybenzoic acid to obtain a second reacted system;
step S3, carrying out a third dehydration condensation reaction on the second reacted system and the humic acid to obtain a third reacted system;
and step S4, carrying out fourth dehydration condensation reaction on the third reacted system and the citric acid and/or the maleic anhydride to obtain a fourth reacted system, namely the sedimentation stabilizer.
8. The method of making according to claim 7, further comprising: and step S5, cooling the fourth reacted system to a certain temperature, and mixing the cooled system with the solvent according to the parts by weight to obtain the settling stabilizer.
9. The preparation method according to claim 7, wherein the temperature of the first dehydration condensation reaction in step S1 is 150-180 ℃ for 3-5 h;
the temperature of the second dehydration condensation reaction in the step S2 is 150-180 ℃, and the time is 2-4 h;
the temperature of the third dehydration condensation reaction in the step S3 is 150-180 ℃, and the time is 2-4 h;
the temperature of the fourth dehydration condensation reaction in the step S4 is 150-180 ℃ and the time is 2-4 h.
10. The method as claimed in claim 8, wherein in step S5, the temperature of the fourth post-reaction system is lowered to 140 ℃ and then mixed with the solvent.
11. Use of the sedimentation stabilizer of any one of claims 4 to 6 in a gas-to-oil synthesis-based drilling fluid system.
12. Use according to claim 11, wherein the gas-to-oil synthesis-based drilling fluid system is used at a temperature below 200 ℃, preferably 120-.
13. The application of claim 11, wherein the oil-water volume ratio of the gas-to-oil synthetic-based drilling fluid system is 70: 30-90: 10.
14. The use of claim 11, wherein the gas-to-oil synthetic-based drilling fluid system has a density of 1.8 to 2.2g/cm 3 。
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