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CN112111039B - Dispersing agent, preparation method and application thereof - Google Patents

Dispersing agent, preparation method and application thereof Download PDF

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Publication number
CN112111039B
CN112111039B CN201910532191.9A CN201910532191A CN112111039B CN 112111039 B CN112111039 B CN 112111039B CN 201910532191 A CN201910532191 A CN 201910532191A CN 112111039 B CN112111039 B CN 112111039B
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temperature
acid
solution
hydrochloric acid
sulfonate
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CN112111039A (en
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王海波
杨小华
杨帆
林永学
金军斌
王琳
李雄
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China Petroleum and Chemical Corp
Sinopec Research Institute of Petroleum Engineering
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Sinopec Research Institute of Petroleum Engineering
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
    • C08F222/02—Acids; Metal salts or ammonium salts thereof, e.g. maleic acid or itaconic acid
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
    • C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F120/04—Acids; Metal salts or ammonium salts thereof
    • C08F120/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/04—Acids; Metal salts or ammonium salts thereof
    • C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/02—Well-drilling compositions
    • C09K8/03—Specific additives for general use in well-drilling compositions
    • C09K8/035—Organic additives
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

Abstract

The invention provides a dispersing agent, a preparation method and application thereof. The preparation method of the dispersant comprises the following steps: 1) mixing water, inorganic acid and unsaturated organic acid, and dissolving at a first temperature to obtain a solution A; 2) adding sulfonate into the solution A under the stirring condition at a second temperature to obtain a solution B; 3) adding an initiator into the solution B at a third temperature to obtain a solution C, introducing nitrogen, and reacting at a fourth temperature to obtain a reaction product; 4) and (3) carrying out suction filtration on the reaction product, drying at a fifth temperature, crushing and sieving to obtain a dry powder dispersing agent.

Description

Dispersing agent, preparation method and application thereof
Technical Field
The invention provides a preparation method of a dispersing agent, in particular to a dispersing agent for drilling fluid.
Background
With the increasing world energy demand, the drilling target gradually turns to the deep stratum, and the probability of drilling the ultra-high temperature and high pressure stratum is higher in the drilling process of the deep stratum. For example, in the United states, the North China sea oil field and other areas, the bottom hole temperature is usually over 200 ℃, the average ground temperature gradient is up to 4.0 ℃/100m, the bottom hole maximum pressure is over 110MPa, and the drilling fluid density during drilling is up to 2.22g/cm3The above; in the Chojia enclosure area in Daqing, the bottom temperature is above 180 ℃, the highest temperature can reach 240 ℃, and the ground temperature gradient can reach 4.1 ℃/100 m; in the domestic south-sea Yingqiong basin, the ground temperature gradient is high, the formation pressure is abnormally high, the maximum temperature of the bottom of a solid drilling well reaches 249 ℃, and the maximum drilling fluid isDensity 2.14g/cm3。
In the deep ultrahigh-temperature and high-pressure stratum environment, the drilling fluid generally has the problems of poor rheological property, difficult regulation, barite settlement and the like, so that underground complexity is caused. The reasons include two points: firstly, the drilling fluid is in a high-temperature condition for a long time, so that clay, drill cuttings and the like in the drilling fluid are dispersed at high temperature, the high-temperature thickening of the drilling fluid is promoted, the viscosity of the drilling fluid is increased, and the rheological property is poor. Secondly, the high-density drilling fluid system means that a large amount of weighting solid phase needs to be added, free water in the system is contended with other treating agents, the high-temperature thickening condition is aggravated, and meanwhile, the viscosity of the system is further increased due to the friction force between solid phase particles.
The effective way for solving the problems is to add a dispersing agent, which is one of the drilling fluid core treating agents and mainly has the functions of breaking up the grid structure among particles in the drilling fluid system and reducing the structural viscosity of the system. The dispersing agent is an ultrahigh-temperature high-density drilling fluid technology as a core element, and has extremely important significance for safely drilling deep ultrahigh-temperature high-pressure stratum, improving drilling speed, reducing cost and improving efficiency.
In recent years, a great deal of research is carried out in China on dispersants suitable for ultrahigh-temperature drilling fluid and ultrahigh-density drilling fluid, and important types comprise lignin, humic acid, organophosphine and organosilicon. Their main role is to reduce the viscosity rise due to clay particles and finely divided solids, and to have limited effect on viscosity rise due to the addition of too much heavy solids in ultra-high density drilling fluids. Meanwhile, the molecules of the treating agent generate radical variation and conformation damage under the condition of ultrahigh temperature, even main chain breakage occurs, and in order to avoid the viscosity of the drilling fluid system from rising again, new dispersing agent needs to be continuously added in use, so that the cost of field construction is increased.
Disclosure of Invention
In order to solve the problems in the prior art, the invention discloses an ultra-high temperature resistant dispersant for high-density drilling fluid and a preparation method thereof, and the product is completely different from the existing lignin dispersants, humic acids dispersants, organic phosphines and organic silicon dispersants. The dispersant prepared by the method is a dispersant,can be heated at 220 ℃ and 2.2g/cm3Reduced viscosity rise in high density systems due to clay particles and finely dispersed solids, and viscosity rise due to low free water in high density drilling fluids and high internal friction of solid weighting materials. Meanwhile, the product can provide a long-acting viscosity reduction effect, the viscosity of the drilling fluid is kept in a reasonable range for a long time, and the construction cost is greatly reduced.
The invention provides a preparation method of a dispersing agent, which comprises the following steps:
1) mixing water, inorganic acid and unsaturated organic acid, and dissolving at a first temperature to obtain a solution A;
2) adding sulfonate into the solution A at a second temperature to obtain a solution B;
3) and adding an initiator into the solution B at a third temperature to obtain a solution C, introducing nitrogen, and reacting at a fourth temperature to obtain a reaction product containing the dispersing agent.
In a particular embodiment, the method further comprises a step 4) after step 3): and (3) carrying out suction filtration on the reaction product, drying at a fifth temperature, crushing and sieving to obtain a dry powder dispersing agent.
In one embodiment, in step 1), water, an inorganic acid, and an unsaturated organic acid are mixed under a first stirring speed condition and dissolved at a first temperature to obtain solution a.
In one embodiment, in step 2), sulfonate is added to solution a at a second temperature and a second stirring speed to obtain solution B.
In one embodiment, in step 3), an initiator is added to solution B at a third temperature and a third stirring speed to obtain solution C.
In one embodiment, the first stirring speed, the second stirring speed, and the third stirring speed are independently 250r/min to 400 r/min.
In one embodiment, in step 4), the pulverization may be performed using a universal pulverizer (model RHP-400, Wanji plastics, Zhejiang).
In one embodiment, in step 4), 16 to 30 mesh screens may be passed. For example, 20 mesh.
In a specific embodiment, the mass percentages of the three monomers of the inorganic acid, the unsaturated organic acid and the sulfonate are 20 to 60 percent, 30 to 60 percent and 10 to 20 percent in sequence, wherein the total mass of the inorganic acid, the unsaturated organic acid and the sulfonate is taken as 100 percent; the amount of the initiator is 0.1 to 0.5 percent.
In one embodiment, the total concentration of the inorganic acid, the unsaturated organic acid and the sulfonate is 23% to 29% (28.6% ≈ 29%) based on 100% of the total mass of the solution C.
In one embodiment, the mineral acid comprises hydrochloric acid and phosphorous acid.
In a specific embodiment, the hydrochloric acid is in a mass ratio of the hydrochloric acid to the phosphorous acid, as hydrogen chloride, of from 1.2:1 to 1.5: 1.
In one embodiment, the unsaturated organic acid includes at least one selected from itaconic acid, acrylic acid, and methacrylic acid.
In one embodiment, the sulfonate salt is sodium sulfonate.
In a specific embodiment, the sulfonate comprises at least one selected from the group consisting of sodium styrene sulfonate, sodium methyl sulfonate, and sodium p-styrene sulfonate.
In one embodiment, the initiator comprises at least one selected from the group consisting of ammonium persulfate, potassium persulfate, and azobisisobutyramidine hydrochloride.
In a specific embodiment, the first temperature, the second temperature, the third temperature, the fourth temperature, and the fifth temperature are independently 60 to 120 ℃;
in a specific embodiment, the first temperature, the second temperature, the third temperature, the fourth temperature, and the fifth temperature are independently 100 to 120 ℃.
In one embodiment, the initiator is added over a period of 10min to 60 min.
In one embodiment, the initiator is added over a period of 10min to 30 min.
In one embodiment, nitrogen is introduced for a reaction time of 1 to 5 hours at the fourth temperature.
In one embodiment, nitrogen is introduced for a reaction time of 1 to 2 hours at the fourth temperature.
In one embodiment, the drying time is from 24 hours to 36 hours.
The second invention provides a dispersant prepared by the preparation method of any one of the first invention.
The third invention provides application of the dispersant prepared by the preparation method in drilling fluid.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary of the invention and are not to be construed as limiting the invention in any way.
Phosphorous acid was purchased from national drug group chemical agents corporation.
Hydrochloric acid was purchased from national pharmaceutical group chemical agents corporation.
Itaconic acid was purchased from Guangzhou science and technology development, Inc., Tianjin.
Acrylic acid was purchased from Beijing chemical industries.
Methacrylic acid was purchased from Beijing chemical plant.
Sodium p-styrenesulfonate was purchased from Zibolidaceae Fine chemical technology, Inc.
Sodium styrene sulfonate was purchased from Zibolidaceae Fine chemical technology, Inc.
Sodium methanesulfonate was purchased from Suning chemical Co., Ltd, Tanzhou.
Ammonium persulfate was purchased from national pharmaceutical group chemical agents corporation.
Potassium persulfate was purchased from the national pharmaceutical group chemicals corporation.
Initiator V-50 was purchased from Kaixin New materials science and technology, Inc., Qingdao.
Sodium carbonate was purchased from the national pharmaceutical group chemical reagent company.
Bentonite was purchased from Bohai drilling mud.
Barite is purchased from Sichuan Huaxi mining Co., Ltd, and has a density of 4.2g/cm3。
Commercial dispersant a: turpan is a firm of Industrial trade, Inc.
Commercially available dispersant B: victory oil field and petroleum technology limited.
The high-density drilling fluid base slurry used in each example has the same formula, and the formula of the high-density drilling fluid base slurry is as follows:
300mL of distilled water was measured and placed in a cup, 0.42g of anhydrous sodium carbonate and 12.0g of bentonite (weighed to 0.01g) were added, and stirring was carried out at high speed for 20min, at least twice during which, to scrape the bentonite adhering to the container wall, after curing was carried out at 25 ℃ for 24h, 756g of barite was added with high speed stirring, then stirring was continued for 10min with high speed, and the base slurry Φ 100 reading was measured with a six-speed rotational viscometer.
And (3) viscosity reduction rate effect evaluation: taking six parts of weighted base slurry, taking one part of base slurry as a blank sample at normal temperature, stirring for 10min at a high speed, and measuring the reading phi of 100 revolutions by using a six-speed rotational viscosity meter100(1)(ii) a 4.8g of the dispersant sample prepared in each example was added to the second portion of the base slurry with stirring by a glass rod, and then stirred at high speed for 10min before measuring 100 revolutions and reading phi100(2)(ii) a Stirring the third base slurry at high speed for 10min, placing in a roller heating furnace, rolling at 220 deg.C for 16h, cooling to 25 deg.C, stirring at high speed for 5min, and measuring the reading phi of 100 revolutions100(3)(ii) a Adding 4.8g of the dispersant sample prepared in each example into the fourth base slurry under the stirring of a glass rod, then stirring at a high speed for 10min, putting into a roller heating furnace, rolling for 16h at 220 ℃, cooling to 25 ℃, stirring at a high speed for 5min, and measuring the reading phi of 100 revolutions100(4). Stirring the fifth base slurry at a high speed for 10min, placing the fifth base slurry into a roller heating furnace, rolling the fifth base slurry at 220 ℃ for 48h, cooling the fifth base slurry to 25 ℃, stirring the fifth base slurry at a high speed for 5min, and measuring the reading phi of 100 revolutions100(5)(ii) a Adding 4.8g of the dispersant sample prepared in each example into the sixth base slurry under stirring of a glass rod, stirring at high speed for 10min, placing into a roller heating furnace, rolling at 220 ℃ for 48h, cooling to 25 ℃, stirring at high speed for 5min, and measuringReading of 100 revolutions phi100(6). The viscosity reduction rate of the dispersant prepared in each example was calculated according to the formula (1), the formula (2) and the formula (3) at room temperature, after aging at 220 ℃/16h and after aging at 220 ℃/48 h.
Figure BDA0002100100550000041
Figure BDA0002100100550000042
Figure BDA0002100100550000043
In the formula:
P1the normal temperature viscosity reduction rate is percent;
P2viscosity reduction rate after aging at 220 ℃/16h is percent;
P3viscosity reduction rate after aging at 220 ℃/48h,%;
Ф100(1)reading the normal temperature base slurry at 100 r/min;
Ф100(2)reading the normal temperature base slurry at 100r/min after sample adding;
Ф100(3)-a reading of 100r/min at 220 ℃/16h base stock;
Ф100(4)after sample loading, reading the base slurry at 220 ℃/16h for 100 r/min;
Ф100(5)-a reading of 100r/min at 220 ℃/48h base stock;
Ф100(6)after sample application, a reading of 100r/min of 220 ℃/48h of base slurry.
Example 1
1. Preparation of ultra-high temperature high density drilling fluid dispersant
1) In a four-necked flask equipped with a stirrer, a dropping funnel, a condenser tube and a thermometer, 12g of hydrochloric acid, 8g of phosphorous acid, 60g of itaconic acid and 333g of water were mixed with stirring at 250r/min, and heated to 60 ℃ to be dissolved, thereby obtaining a solution A;
2) dropwise adding 20g of sodium styrene sulfonate into the solution A at the temperature of 60 ℃ under the stirring condition of 250r/min to obtain solution B;
3) dropwise adding 0.1g of ammonium persulfate into the solution B under the stirring condition of 250r/min at the temperature of 60 ℃, finishing the addition of the ammonium persulfate within 10min to obtain a solution C, introducing nitrogen at the temperature of 60 ℃ for heat preservation reaction for 1 hour, and cooling to obtain a product;
4) and (3) carrying out suction filtration and drying on the product, crushing the product by using a universal crusher (RHP-400 type, Wanji plastic industries, Zhejiang), and sieving the crushed product by using a 16-mesh sieve to prepare the dry powder dispersing agent for the ultrahigh-temperature high-density drilling fluid system. Wherein the drying temperature is: drying time was 24 hours at 60 ℃.
Taking the total mass of hydrochloric acid, phosphorous acid, itaconic acid and sodium styrene sulfonate as 100%, the mass sum of the hydrochloric acid and the phosphorous acid accounts for 20%, the mass sum of the itaconic acid accounts for 60%, and the mass sum of the sodium styrene sulfonate accounts for 20%; the amount of initiator used was 0.1%. The mass ratio of hydrochloric acid to phosphorous acid was 12:8 to 1.5: 1. Wherein the mass of the hydrochloric acid is calculated by hydrogen chloride.
The total concentration of hydrochloric acid, phosphorous acid, itaconic acid and sodium styrene sulfonate was 23% (100/(100+333)) based on the total mass of solution C being 100%.
2. Evaluation of viscosity reduction Effect
The results are shown in Table 1.
Example 2
1. Preparation of ultra-high temperature high density drilling fluid dispersant
1) In a four-necked flask equipped with a stirrer, a dropping funnel, a condenser tube and a thermometer, 10.91g of hydrochloric acid, 9.09g of phosphorous acid, 60g of itaconic acid and 333g of water were mixed under stirring at 400r/min, and heated to 100 ℃ to be dissolved, to obtain a solution A;
2) dropwise adding 20g of sodium styrene sulfonate into the solution A at the temperature of 100 ℃ under the stirring condition of 400r/min to obtain solution B;
3) dropwise adding 0.1g of ammonium persulfate into the solution B under the stirring condition of 400r/min at the temperature of 100 ℃, finishing the addition of the ammonium persulfate within 60min to obtain a solution C, introducing nitrogen at the temperature of 100 ℃ for heat preservation reaction for 5 hours, and cooling to obtain a product;
4) the product is filtered, dried, crushed by a universal crusher (RHP-400 type, manufactured by Wanji plastic industries, Zhejiang) and sieved by a 30-mesh sieve to prepare the dry powder dispersing agent for the ultrahigh-temperature high-density drilling fluid system. Wherein the drying temperature is: drying time was 36 hours at 100 ℃.
Taking the total mass of hydrochloric acid, phosphorous acid, itaconic acid and sodium styrene sulfonate as 100%, the total mass of hydrochloric acid and phosphorous acid is 20%, the mass of itaconic acid is 60%, and the mass of sodium styrene sulfonate is 20%; the initiator is used in an amount of 0.1%. The mass ratio of hydrochloric acid to phosphorous acid was 10.91:9.09 to 1.2: 1. Wherein the mass of the hydrochloric acid is calculated by hydrogen chloride.
The total concentration of hydrochloric acid, phosphorous acid, itaconic acid and sodium styrene sulfonate was 23% (100/(100+333)) based on the total mass of solution C being 100%.
2. Evaluation of viscosity reduction Effect
The results are shown in Table 1.
Example 3
1) In a four-necked flask equipped with a stirrer, a dropping funnel, a condenser tube and a thermometer, 11.45g of hydrochloric acid, 8.55g of phosphorous acid, 60g of itaconic acid and 333g of water were mixed under stirring at 300r/min, and heated to 120 ℃ to be dissolved, to obtain a solution A;
2) dropwise adding 20g of sodium styrene sulfonate into the solution A at 120 ℃ under the stirring condition of 300r/min to obtain solution B;
3) dropwise adding 0.1g of ammonium persulfate into the solution B under the stirring condition of 300r/min at 120 ℃, finishing the addition of the ammonium persulfate within 10min to obtain a solution C, introducing nitrogen at 120 ℃ for heat preservation reaction for 1 hour, and cooling to obtain a product;
4) the product is filtered, dried, crushed by a universal crusher (RHP-400 type, manufactured by Wanji plastic industries, Zhejiang) and sieved by a 20-mesh sieve to prepare the dry powder dispersing agent for the ultrahigh-temperature high-density drilling fluid system. Wherein the drying temperature is: drying time was 24 hours at 120 ℃.
Taking the total mass of hydrochloric acid, phosphorous acid, itaconic acid and sodium styrene sulfonate as 100%, the total mass of hydrochloric acid and phosphorous acid is 20%, the mass of itaconic acid is 60%, and the mass of sodium styrene sulfonate is 20%; the amount of initiator used was 0.1%. The mass ratio of hydrochloric acid to phosphorous acid was 229:171 to 1.34: 1. Wherein the mass of the hydrochloric acid is calculated by hydrogen chloride.
The total concentration of hydrochloric acid, phosphorous acid, itaconic acid and sodium styrenesulfonate was 23% (100/(100+333)) with respect to the total mass of the solution C being 100%.
2. Evaluation of viscosity reduction Effect
The results are shown in Table 1.
Example 4
1. Preparation of ultra-high temperature high density drilling fluid dispersant
1) In a four-necked flask equipped with a stirrer, a dropping funnel, a condenser tube and a thermometer, 11.45g of hydrochloric acid, 8.55g of phosphorous acid, 60g of itaconic acid and 333g of water were mixed under stirring at 300r/min, and heated to 100 ℃ to be dissolved, to obtain a solution A;
2) dropwise adding 20g of sodium styrene sulfonate into the solution A at 100 ℃ under the stirring condition of 300r/min to obtain solution B;
3) dropwise adding 0.1g of ammonium persulfate into the solution B under the stirring condition of 300r/min at 120 ℃, finishing the addition of the ammonium persulfate within 30min to obtain a solution C, introducing nitrogen at 120 ℃ for heat preservation reaction for 2 hours, and cooling to obtain a product;
4) the product is filtered, dried, crushed by a universal crusher (RHP-400 type, manufactured by Wanji plastic industries, Zhejiang) and sieved by a 20-mesh sieve to prepare the dry powder dispersing agent for the ultrahigh-temperature high-density drilling fluid system. Wherein the drying temperature is: drying time was 36 hours at 120 ℃.
Taking the total mass of hydrochloric acid, phosphorous acid, itaconic acid and sodium styrene sulfonate as 100%, the mass sum of the hydrochloric acid and the phosphorous acid accounts for 20%, the mass sum of the itaconic acid accounts for 60%, and the mass sum of the sodium styrene sulfonate accounts for 20%; the amount of initiator used was 0.1%. The mass ratio of hydrochloric acid to phosphorous acid was 229:171 to 1.34: 1. Wherein the mass of the hydrochloric acid is calculated by hydrogen chloride.
The total concentration of hydrochloric acid, phosphorous acid, itaconic acid and sodium styrene sulfonate was 23% (100/(100+333)) based on the total mass of solution C being 100%.
2. Evaluation of viscosity reduction Effect
The results are shown in Table 1.
Example 5
1. Preparation of ultra-high temperature high density drilling fluid dispersant
1) In a four-necked flask equipped with a stirrer, a dropping funnel, a condenser tube and a thermometer, 36g of hydrochloric acid, 24g of phosphorous acid, 30g of acrylic acid and 250g of water were mixed under stirring at 300r/min, and heated to 60 ℃ to be dissolved, thereby obtaining a solution A;
2) dropwise adding 10g of sodium methanesulfonate into the solution A at 60 ℃ under the stirring condition of 300r/min to obtain a solution B;
3) dropwise adding 0.5g of potassium persulfate into the solution B under the stirring condition of 300r/min at the temperature of 60 ℃, finishing adding the potassium persulfate within 10min to obtain a solution C, introducing nitrogen at the temperature of 60 ℃, carrying out heat preservation reaction for 1 hour, and cooling to obtain a product;
4) the product is filtered, dried, crushed by a universal crusher (RHP-400 type, manufactured by Wanji plastic industries, Zhejiang) and sieved by a 20-mesh sieve to prepare the dry powder dispersing agent for the ultrahigh-temperature high-density drilling fluid system. Wherein the drying temperature is: drying time was 24 hours at 60 ℃.
Taking the total mass of the hydrochloric acid, the phosphorous acid, the acrylic acid and the sodium methanesulfonate as 100 percent, the total mass of the hydrochloric acid and the phosphorous acid accounts for 60 percent, the acrylic acid accounts for 30 percent and the sodium methanesulfonate accounts for 10 percent; the amount of initiator used was 0.5%. The mass ratio of hydrochloric acid to phosphorous acid was 36:24 to 1.5: 1. Wherein the mass of the hydrochloric acid is calculated by hydrogen chloride.
The total concentration of hydrochloric acid, phosphorous acid, acrylic acid and sodium methanesulfonate was 28.6% (100/(100+250)) based on the total mass of solution C being 100%.
2. Evaluation of viscosity reduction Effect
The results are shown in Table 1.
Example 6
1) 32.73g of hydrochloric acid, 27.27g of phosphorous acid, 30g of acrylic acid and 250g of water were mixed with stirring at 300r/min in a four-necked flask equipped with a stirrer, a dropping funnel, a condenser and a thermometer, and heated to 100 ℃ to dissolve them, thereby obtaining a solution A;
2) dropwise adding 10g of sodium methanesulfonate into the solution A at 100 ℃ under the stirring condition of 300r/min to obtain a solution B;
3) dropwise adding 0.5g of potassium persulfate into the solution B under the stirring condition of 300r/min at the temperature of 100 ℃, finishing adding the potassium persulfate within 60min to obtain a solution C, introducing nitrogen at the temperature of 100 ℃ for heat preservation reaction for 5 hours, and cooling to obtain a product;
4) the product is filtered, dried, crushed by a universal crusher (RHP-400 type, manufactured by Wanji plastic industries, Zhejiang) and sieved by a 20-mesh sieve to prepare the dry powder dispersing agent for the ultrahigh-temperature high-density drilling fluid system. Wherein the drying temperature is: drying time was 36 hours at 100 ℃.
Taking the total mass of the hydrochloric acid, the phosphorous acid, the acrylic acid and the sodium methanesulfonate as 100 percent, the total mass of the hydrochloric acid and the phosphorous acid accounts for 60 percent, the acrylic acid accounts for 30 percent and the sodium methanesulfonate accounts for 10 percent; the amount of initiator used was 0.5%. The mass ratio of hydrochloric acid to phosphorous acid was 32.73:27.27 to 1.2: 1. Wherein the mass of the hydrochloric acid is calculated by hydrogen chloride.
The total concentration of hydrochloric acid, phosphorous acid, acrylic acid and sodium methanesulfonate was 28.6% (100/(100+250)) based on the total mass of solution C being 100%.
2. Evaluation of viscosity reduction Effect
The results are shown in Table 1.
Example 7
1. Preparation of ultra-high temperature high density drilling fluid dispersant
1) In a four-necked flask equipped with a stirrer, a dropping funnel, a condenser tube and a thermometer, 34.36g of hydrochloric acid, 25.64g of phosphorous acid, 30g of acrylic acid and 250g of water were mixed under stirring at 300r/min, and heated to 120 ℃ to be dissolved, thereby obtaining a solution A;
2) dropwise adding 10g of sodium methanesulfonate into the solution A at 120 ℃ under the stirring condition of 300r/min to obtain a solution B;
3) dropwise adding 0.5g of potassium persulfate into the solution B under the stirring condition of 300r/min at 120 ℃, finishing adding the potassium persulfate within 10min to obtain a solution C, introducing nitrogen at 120 ℃ for heat preservation reaction for 1 hour, and cooling to obtain a product;
4) the product is filtered, dried, crushed by a universal crusher (RHP-400 type, manufactured by Wanji plastic industries, Zhejiang) and sieved by a 20-mesh sieve to prepare the dry powder dispersing agent for the ultrahigh-temperature high-density drilling fluid system. Wherein the drying temperature is: drying time was 24 hours at 120 ℃.
Taking the total mass of the hydrochloric acid, the phosphorous acid, the acrylic acid and the sodium methanesulfonate as 100%, the total mass of the hydrochloric acid and the phosphorous acid accounts for 60%, the mass of the acrylic acid accounts for 30% and the mass of the sodium methanesulfonate accounts for 10%; the amount of initiator used was 0.5%. The mass ratio of hydrochloric acid to phosphorous acid was 34.36:25.64 to 1.34: 1. Wherein the mass of the hydrochloric acid is calculated by hydrogen chloride.
The total concentration of hydrochloric acid, phosphorous acid, acrylic acid and sodium methanesulfonate was 28.6% (100/(100+250)) based on the total mass of solution C being 100%.
2. Evaluation of viscosity reduction Effect
The results are shown in Table 1.
Example 8
1. Preparation of ultra-high temperature high density drilling fluid dispersant
1) In a four-necked flask equipped with a stirrer, a dropping funnel, a condenser tube and a thermometer, 34.36g of hydrochloric acid, 25.64g of phosphorous acid, 30g of acrylic acid and 250g of water were mixed under stirring at 300r/min, and heated to 100 ℃ to be dissolved, to obtain a solution A;
2) dropwise adding 10g of sodium methanesulfonate into the solution A at 100 ℃ under the stirring condition of 300r/min to obtain a solution B;
3) dropwise adding 0.5g of potassium persulfate into the solution B under the stirring condition of 300r/min at 120 ℃, finishing adding the potassium persulfate within 30min to obtain a solution C, introducing nitrogen at 120 ℃ for heat preservation reaction for 2 hours, and cooling to obtain a product;
4) the product is filtered, dried, crushed by a universal crusher (RHP-400 type, manufactured by Wanji plastic industries, Zhejiang) and sieved by a 20-mesh sieve to prepare the dry powder dispersing agent for the ultrahigh-temperature high-density drilling fluid system. Wherein the drying temperature is: drying time was 36 hours at 120 ℃.
Taking the total mass of the hydrochloric acid, the phosphorous acid, the acrylic acid and the sodium methanesulfonate as 100 percent, the total mass of the hydrochloric acid and the phosphorous acid accounts for 60 percent, the acrylic acid accounts for 30 percent and the sodium methanesulfonate accounts for 10 percent; the amount of initiator used was 0.5%. The mass ratio of hydrochloric acid to phosphorous acid was 229:171 to 1.34: 1. Wherein the mass of the hydrochloric acid is calculated by hydrogen chloride.
The total concentration of hydrochloric acid, phosphorous acid, acrylic acid and sodium methanesulfonate was 28.6% (100/(100+250)) based on the total mass of solution C as 100%. 2. Evaluation of viscosity reduction Effect
The results are shown in Table 1.
Example 9
1. Preparation of ultra-high temperature high density drilling fluid dispersant
1) In a four-necked flask equipped with a stirrer, a dropping funnel, a condenser and a thermometer, 34.36g of hydrochloric acid, 25.64g of phosphorous acid, 30g of methacrylic acid and 250g of water were mixed under stirring at 300r/min, and heated to 60 ℃ to be dissolved, thereby obtaining a solution A;
2) dropwise adding 10g of sodium p-styrene sulfonate into the solution A at 60 ℃ under the stirring condition of 300r/min to obtain solution B;
3) dropwise adding 0.1g V-50 into the solution B under the stirring condition of 300r/min at 60 ℃, completely adding potassium persulfate within 10min to obtain a solution C, introducing nitrogen at 60 ℃ for heat preservation reaction for 1 hour, and cooling to obtain a product;
4) the product is filtered, dried, crushed by a universal crusher (RHP-400 type, manufactured by Wanji plastic industries, Zhejiang) and sieved by a 20-mesh sieve to prepare the dry powder dispersing agent for the ultrahigh-temperature high-density drilling fluid system. Wherein the drying temperature is: drying time was 24 hours at 60 ℃.
Taking the total mass of the hydrochloric acid, the phosphorous acid, the methacrylic acid and the sodium p-styrene sulfonate as 100%, the total mass of the hydrochloric acid and the phosphorous acid accounts for 60%, the mass of the methacrylic acid accounts for 30%, and the mass of the sodium p-styrene sulfonate accounts for 10%; the amount of initiator used was 0.1%. The mass ratio of hydrochloric acid to phosphorous acid was 229:171 to 1.34: 1. Wherein the mass of the hydrochloric acid is calculated by hydrogen chloride.
The total concentration of hydrochloric acid, phosphorous acid, methacrylic acid and sodium p-styrenesulfonate was 28.6% (100/(100+250)) based on 100% of the total mass of solution C.
2. Evaluation of viscosity reduction Effect
The results are shown in Table 1.
Example 10
1. Preparation of ultra-high temperature high density drilling fluid dispersant
1) In a four-necked flask equipped with a stirrer, a dropping funnel, a condenser and a thermometer, 34.36g of hydrochloric acid, 25.64g of phosphorous acid, 30g of methacrylic acid and 250g of water were mixed under stirring at 300r/min, and heated to 100 ℃ to be dissolved, to obtain a solution A;
2) dropwise adding 10g of sodium p-styrene sulfonate into the solution A at 100 ℃ under the stirring condition of 300r/min to obtain a solution B;
3) dropwise adding 0.1g V-50 into the solution B under the stirring condition of 300r/min at 100 ℃, completely adding potassium persulfate within 60min to obtain a solution C, introducing nitrogen at 100 ℃ for heat preservation reaction for 5 hours, and cooling to obtain a product;
4) the product is filtered, dried, crushed by a universal crusher (RHP-400 type, manufactured by Wanji plastic industries, Zhejiang) and sieved by a 20-mesh sieve to prepare the dry powder dispersing agent for the ultrahigh-temperature high-density drilling fluid system. Wherein the drying temperature is as follows: drying time was 36 hours at 100 ℃.
Taking the total mass of the hydrochloric acid, the phosphorous acid, the methacrylic acid and the sodium p-styrene sulfonate as 100%, the total mass of the hydrochloric acid and the phosphorous acid accounts for 60%, the mass of the methacrylic acid accounts for 30%, and the mass of the sodium p-styrene sulfonate accounts for 10%; the amount of initiator used was 0.1%. The mass ratio of hydrochloric acid to phosphorous acid was 229:171 to 1.34: 1. Wherein the mass of the hydrochloric acid is calculated by hydrogen chloride.
The total concentration of hydrochloric acid, phosphorous acid, methacrylic acid and sodium p-styrenesulfonate was 28.6% (100/(100+250)) based on 100% of the total mass of solution C.
2. Evaluation of viscosity reduction Effect
The results are shown in Table 1.
Example 11
1. Preparation of ultra-high temperature high density drilling fluid dispersant
1) In a four-necked flask equipped with a stirrer, a dropping funnel, a condenser and a thermometer, 34.36g of hydrochloric acid, 25.64g of phosphorous acid, 30g of methacrylic acid and 250g of water were mixed under stirring at 300r/min, and heated to 120 ℃ to be dissolved, thereby obtaining a solution A;
2) dropwise adding 10g of sodium p-styrene sulfonate into the solution A at 120 ℃ under the stirring condition of 300r/min to obtain solution B;
3) dropwise adding 0.1g V-50 into the solution B under the stirring condition of 300r/min at 120 ℃, completely adding potassium persulfate within 10min to obtain a solution C, introducing nitrogen at 120 ℃ for heat preservation reaction for 1 hour, and cooling to obtain a product;
4) the product is filtered, dried, crushed by a universal crusher (RHP-400 type, manufactured by Wanji plastic industries, Zhejiang) and sieved by a 20-mesh sieve to prepare the dry powder dispersing agent for the ultrahigh-temperature high-density drilling fluid system. Wherein the drying temperature is: drying time was 24 hours at 120 ℃.
Taking the total mass of the hydrochloric acid, the phosphorous acid, the methacrylic acid and the sodium p-styrene sulfonate as 100%, the total mass of the hydrochloric acid and the phosphorous acid accounts for 60%, the mass of the methacrylic acid accounts for 30%, and the mass of the sodium p-styrene sulfonate accounts for 10%; the amount of initiator used was 0.1%. The mass ratio of hydrochloric acid to phosphorous acid was 229:171 to 1.34: 1. Wherein the mass of the hydrochloric acid is calculated by hydrogen chloride.
The total concentration of hydrochloric acid, phosphorous acid, methacrylic acid and sodium p-styrenesulfonate was 28.6% (100/(100+250)) based on 100% of the total mass of solution C.
2. Evaluation of viscosity reduction Effect
The results are shown in Table 1.
Example 12
1. Preparation of ultra-high temperature high density drilling fluid dispersant
1) In a four-necked flask equipped with a stirrer, a dropping funnel, a condenser and a thermometer, 34.36g of hydrochloric acid, 25.64g of phosphorous acid, 30g of methacrylic acid and 250g of water were mixed under stirring at 300r/min, and heated to 100 ℃ to be dissolved, to obtain a solution A;
2) dropwise adding 10g of sodium p-styrene sulfonate into the solution A at 100 ℃ under the stirring condition of 300r/min to obtain a solution B;
3) dropwise adding 0.1g V-50 into the solution B at 120 ℃ under the stirring condition of 300r/min, completely adding potassium persulfate within 30min to obtain a solution C, introducing nitrogen at 120 ℃ for heat preservation reaction for 2 hours, and cooling to obtain a product;
4) the product is filtered, dried, crushed by a universal crusher (RHP-400 type, manufactured by Wanji plastic industries, Zhejiang) and sieved by a 20-mesh sieve to prepare the dry powder dispersing agent for the ultrahigh-temperature high-density drilling fluid system. Wherein the drying temperature is: drying time was 36 hours at 120 ℃.
Taking the total mass of the hydrochloric acid, the phosphorous acid, the methacrylic acid and the sodium p-styrene sulfonate as 100%, the total mass of the hydrochloric acid and the phosphorous acid accounts for 60%, the mass of the methacrylic acid accounts for 30%, and the mass of the sodium p-styrene sulfonate accounts for 10%; the amount of initiator used was 0.1%. The mass ratio of hydrochloric acid to phosphorous acid was 229:171 to 1.34: 1. Wherein the mass of the hydrochloric acid is calculated by hydrogen chloride.
The total concentration of hydrochloric acid, phosphorous acid, methacrylic acid and sodium p-styrenesulfonate was 28.6% (100/(100+250)) based on 100% of the total mass of solution C.
2. Evaluation of viscosity reduction Effect
The results are shown in Table 1.
Comparative example 1
The commercial dispersant A was used as a control for evaluating the effect of viscosity reduction. The results are shown in Table 1.
Comparative example 2
The viscosity reducing effect was evaluated by using a commercially available dispersant B as a control. The results are shown in Table 1.
TABLE 1 evaluation results of viscosity reduction ratio in examples
Figure BDA0002100100550000121
As can be seen from experimental data, after the dispersant for the drilling fluid is added, the content of the dispersant is 2.20g/cm3The reading of the drilling fluid base slurry is greatly reduced at 100 revolutions, the viscosity reduction rate can reach 83.6 percent at most, and the viscosity reduction rate is higher than that of the conventional commercially available dispersants A and B. After rolling aging is carried out for 16h at 220 ℃, the highest viscosity reduction rate of the dispersant for the drilling fluid is still more than 60%, which shows that the dispersant has good dispersion effect on the high-density solid-phase weighting agent at ultrahigh temperature. After the conventional dispersants A and B sold in the market are subjected to rolling aging at 220 ℃ for 16 hours, the viscosity reduction rate is reduced in response, and even no effect is generated, which shows that partial decomposition products are completely decomposed after the two dispersants are subjected to rolling aging at 220 ℃ for 16 hours. After rolling aging at 220 ℃ for 48 hours, the dispersant for drilling fluid added in the invention still has higher viscosity reduction and dispersion capability, which shows that the dispersant has long-acting viscosity reduction effect, and in actual construction, the rheological property of the drilling fluid can be ensured to be stable for a long time without frequent addition, and the construction cost can be greatly reduced. Both conventional commercial dispersants did not have any viscosity reducing effect after 48h at 220 ℃.
While the present application has been described with reference to specific embodiments, those skilled in the art will appreciate that various changes can be made without departing from the true spirit and scope of the present application. In addition, many modifications may be made to adapt a particular situation, material, composition of matter, and method to the objective, spirit and scope of the present application. All such modifications are intended to be included within the scope of the claims of this application.

Claims (13)

1. A preparation method of a dispersing agent comprises the following steps:
1) mixing water, inorganic acid and unsaturated organic acid, and dissolving at a first temperature to obtain a solution A; the inorganic acid comprises hydrochloric acid and phosphorous acid; the hydrochloric acid is calculated by hydrogen chloride, and the mass ratio of the hydrochloric acid to the phosphorous acid is 1.2:1 to 1.5: 1; the unsaturated organic acid comprises at least one selected from itaconic acid, acrylic acid and methacrylic acid;
2) adding sulfonate into the solution A at a second temperature to obtain a solution B; the sulfonate comprises at least one of sodium styrene sulfonate and sodium p-styrene sulfonate;
3) adding an initiator into the solution B at a third temperature to obtain a solution C, introducing nitrogen, and reacting at a fourth temperature to obtain a reaction product containing the dispersing agent; the fourth temperature is 60 to 120 ℃, and the reaction time of introducing nitrogen at the fourth temperature is 1 to 5 hours; the total concentration of the inorganic acid, the unsaturated organic acid and the sulfonate is 23 to 29 percent based on the total mass of the solution C as 100 percent;
taking the total mass of the inorganic acid, the unsaturated organic acid and the sulfonate as 100%, wherein the mass percentages of the inorganic acid, the unsaturated organic acid and the sulfonate are 20-60%, 30-60% and 10-20% in sequence; the amount of the initiator is 0.1 to 0.5 percent.
2. The method of manufacturing according to claim 1, further comprising step 4) after step 3): and (3) carrying out suction filtration on the reaction product, drying at a fifth temperature, crushing and sieving to obtain a dry powder dispersing agent.
3. The production method according to claim 1 or 2, characterized in that the initiator comprises at least one selected from the group consisting of ammonium persulfate, potassium persulfate, and azobisisobutyramidine hydrochloride.
4. The production method according to claim 1 or 2, characterized in that the first temperature, the second temperature, and the third temperature are independently 60 to 120 ℃.
5. The production method according to claim 1 or 2, characterized in that the first temperature, the second temperature, the third temperature, and the fourth temperature are independently 100 to 120 ℃.
6. The method of claim 2, wherein the fifth temperature is 60 to 120 ℃.
7. The method of claim 2, wherein the fifth temperature is 100 to 120 ℃.
8. A method according to claim 1 or 2, characterized in that the initiator addition is completed within 10min to 60 min.
9. A method according to claim 1 or 2, characterized in that the initiator addition is completed within 10min to 30 min.
10. The method according to claim 1 or 2, wherein the reaction time at the fourth temperature by introducing nitrogen is 1 to 2 hours.
11. The method according to claim 2, wherein the drying time is 24 to 36 hours.
12. A dispersant prepared by the method of any one of claims 1 to 11.
13. Use of the dispersant prepared by the preparation method according to any one of claims 1 to 11 in drilling fluids.
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EP1439195A2 (en) * 1996-07-19 2004-07-21 Coatex S.A.S. Water soluble polymers with low content of residual monomers and their use
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CN107828016A (en) * 2017-11-14 2018-03-23 江苏师范大学 A kind of preparation method of viscosity depressant for drilling fluid

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EP1439195A2 (en) * 1996-07-19 2004-07-21 Coatex S.A.S. Water soluble polymers with low content of residual monomers and their use
CN104312548A (en) * 2014-08-22 2015-01-28 中国石油化工集团公司 Phosphorus-containing high-temperature-resistant drilling-fluid viscosity reducer and preparation method thereof
CN107828016A (en) * 2017-11-14 2018-03-23 江苏师范大学 A kind of preparation method of viscosity depressant for drilling fluid

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