CN109054790B - Hydrate inhibitor and preparation method and application thereof - Google Patents
Hydrate inhibitor and preparation method and application thereof Download PDFInfo
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- CN109054790B CN109054790B CN201811011764.5A CN201811011764A CN109054790B CN 109054790 B CN109054790 B CN 109054790B CN 201811011764 A CN201811011764 A CN 201811011764A CN 109054790 B CN109054790 B CN 109054790B
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- 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
- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17D—PIPE-LINE SYSTEMS; PIPE-LINES
- F17D1/00—Pipe-line systems
- F17D1/08—Pipe-line systems for liquids or viscous products
- F17D1/16—Facilitating the conveyance of liquids or effecting the conveyance of viscous products by modification of their viscosity
- F17D1/17—Facilitating the conveyance of liquids or effecting the conveyance of viscous products by modification of their viscosity by mixing with another liquid, i.e. diluting
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- 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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/22—Hydrates inhibition by using well treatment fluids containing inhibitors of hydrate formers
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Abstract
The invention provides a hydrate inhibitor, which consists of the following components in percentage by weight: 10-50% of terpolymer, 45-85% of ether cosolvent and 1-30% of dispersant; wherein the terpolymer is a terpolymer of vinyl pyrrolidone, vinyl caprolactam and isopropyl methacrylamide; the dispersant is at least one of methylcellulose, sodium carboxymethylcellulose and hydroxyethyl cellulose. Meanwhile, a preparation method and application of the hydrate inhibitor are also provided. The hydrate inhibitor provided by the invention can be used for inhibiting the generation of natural gas hydrate in the gas field exploitation, treatment and transportation processes, and has the advantages of obvious inhibition effect, small usage amount and small harm to the environment.
Description
Technical Field
The invention belongs to the technical field of oil and gas fields, and particularly relates to a hydrate inhibitor and a preparation method and application thereof.
Background
The components such as methane, ethane and carbon dioxide in the natural gas react with water at low temperature and high pressure to generate an ice-crystal solid hydrate, and after the ice-crystal solid hydrate is coalesced, the flow area of a pipeline can be reduced, throttling is generated, and the generation of the hydrate is further accelerated, so that the pipeline and equipment in the processes of gas field exploitation, natural gas treatment and transportation are blocked, and the safe operation of exploitation, transportation and processing of the natural gas is seriously influenced. Therefore, it is important to add inhibitors to prevent and prevent the natural gas from forming hydrates during the production, treatment and transportation process to block the well bore, treatment equipment and gas transmission lines.
The traditional method for inhibiting the formation of natural gas hydrate is to inject thermodynamic inhibitors, such as electrolyte, methanol, glycol and the like, and avoid and inhibit the formation of the hydrate by changing the thermodynamic conditions of the formation of the hydrate. However, the thermodynamic inhibitor has the disadvantages of high use concentration (mass fraction usually accounts for 20-60% of the water phase), high consumption, high cost, high toxicity and the like. Compared with the prior art, the kinetic inhibitor has the advantages of small addition amount, low cost, low toxicity and the like, and thus becomes a hot point of domestic and foreign research. The natural gas aerodynamic inhibitor achieves the purpose of inhibiting by prolonging the nucleation time of the natural gas hydrate or inhibiting the growth of the natural gas hydrate. Research shows that the existing single type low-dose kinetic inhibitor has limited inhibition effect and cannot meet the actual requirement, so that the addition of an auxiliary agent to enhance the inhibition performance of the kinetic inhibitor is a focus of attention.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a hydrate inhibitor and a preparation method thereof, wherein the hydrate inhibitor can effectively inhibit the generation of natural gas hydrate in the process of gas field exploitation and transportation, and has long inhibition time.
A hydrate inhibitor comprises the following components in percentage by weight: 10-50% of terpolymer, 45-85% of ether cosolvent and 1-30% of dispersant;
wherein the terpolymer is prepared from vinyl pyrrolidone, vinyl caprolactam and isopropyl-methacrylamide;
the dispersant is at least one of methylcellulose, sodium carboxymethylcellulose and hydroxyethyl cellulose.
Preferably, the average molecular weight of the terpolymer is 10000-18000 g/mol.
Preferably, the ether cosolvent is any one of propylene glycol methyl ether, propylene glycol ethyl ether and propylene glycol butyl ether.
The preparation method of the hydrate inhibitor comprises the following steps:
(1) preparing a terpolymer;
(2) and then mixing and stirring the terpolymer, the ether cosolvent and the dispersant.
Preferably, the method for preparing the terpolymer in the step (1) is as follows: according to a molar ratio (1-25): (1-85): (1-10) adding three monomers of vinyl pyrrolidone, vinyl caprolactam and isopropyl-methacrylamide and an initiator into an alcohol solvent, and introducing N2After deoxidization, stirring and reacting for 5-16h at 40-85 ℃, cooling to room temperature, standing for 2-3h in an oven at 40-50 ℃, filtering, washing filter residues for 3 times by using water, and drying in a vacuum drying oven to constant weight to obtain the product; wherein, the volume ratio of the total volume of the three monomers to the alcohol solvent is 1: (3-5); the mass ratio of the total mass of the three monomers to the initiator is 1: (3-5).
Preferably, the alcohol solvent is at least two of acetone, methanol, ethanol, propanol, n-butanol and tert-butanol.
Preferably, the initiator is hydrogen peroxide, sodium persulfate, potassium persulfate, or dimethyl azodiisobutyrate.
The application of the hydrate inhibitor is to add the hydrate inhibitor into produced water of an oil and gas field for inhibiting the generation of the hydrate, and specifically comprises the following steps: adding the hydrate inhibitor into produced water of an oil-gas field according to the mass concentration of 0.1-1% under the pressure of 7.0MPa and at the temperature of 2-4 ℃.
The invention has the advantages that:
according to the hydrate inhibitor provided by the invention, the terpolymer is used as a kinetic inhibitor, the ether cosolvent not only can enhance the solubility of the hydrate inhibitor, but also has a thermodynamic inhibition effect and can enhance the inhibition effect, and compared with most of the conventional low-molecular-weight thermodynamic inhibitors, the hydrate inhibitor is lower in toxicity; the dispersing agent can effectively disperse hydrate particles formed in a liquid phase to keep the hydrate particles in a flowing state, so that hydrate blockage is prevented, and the inhibiting effect is synergistically enhanced. Can be used for inhibiting the generation of natural gas hydrate in the process of gas field exploitation, treatment and transportation, and has the advantages of obvious inhibiting effect, small using amount and small harm to the environment.
Detailed Description
Evaluation method of inhibitory effect:
first, the reaction kettle was washed with distilled water, and the washing liquid was discharged. Then pumping a certain amount of experimental water as produced water of an oil and gas field (the degree of mineralization is 52163 mg/L), and pumping air in the reaction kettle away by using a vacuum pump; reaction conditions are as follows: at the temperature of 3 ℃ and the pressure of 7 MPa, 94.83 percent of methane, 0.59 percent of ethane, 0.11 percent of propane and N are introduced21.90%、CO22.57 percent of experimental gas is used, the pressure in the reaction kettle is adjusted to the experimental pressure of 7 MPa, the stirring reaction is carried out at 1000r/min, the experiment is stopped after the pressure in the reaction kettle changes suddenly, the generation process of the hydrate is judged according to the pressure change in the reaction kettle and the temperature condition, and the effect of the inhibitor is evaluated.
Example 1
1. A hydrate inhibitor comprises the following components in percentage by weight: 10% of terpolymer, 85% of ether cosolvent and 5% of dispersant;
wherein the dispersant is methyl cellulose; the ether cosolvent is propylene glycol methyl ether;
the terpolymer is a terpolymer of vinyl pyrrolidone, vinyl caprolactam and isopropyl-methacrylamide, and the average molecular weight is 10000-18000 g/mol;
2. the preparation method of the hydrate inhibitor comprises the following steps:
(1) preparation of the terpolymer: according to a molar ratio of 1: 1: 1 adding three monomers of vinyl pyrrolidone, vinyl caprolactam and isopropyl-methacrylamide and an initiator into an alcohol solvent, and introducing N2After deoxidization, stirring and reacting for 5h at 85 ℃, cooling to room temperature, standing in a drying oven at 40 ℃ for 3h, filtering, washing filter residues with water for 3 times, and drying in a vacuum drying oven to constant weight to obtain the terpolymer of vinyl pyrrolidone, vinyl caprolactam and isopropyl-methacrylamide; wherein the alcohol solvent is a mixed solution of acetone and methanol(ii) a The initiator is hydrogen peroxide; the volume ratio of the total volume of the three monomers to the alcohol solvent is 1: 3; the mass ratio of the total mass of the three monomers to the initiator is 1: 3;
(2) the terpolymer, the ether cosolvent and the dispersant are mixed and stirred.
3. Preparing the inhibitor into a gas field produced aqueous solution with the mass concentration of 0.1%, loading the aqueous solution into a reaction kettle, starting a test under the conditions that the test pressure is 7.0MPa and the test temperature is 3 ℃, and measuring the inhibition time of the generation of the natural gas hydrate to be 4380 min.
Example 2
1. A hydrate inhibitor comprises the following components in percentage by weight: 50% of terpolymer, 49% of ether cosolvent and 1% of dispersant;
wherein the dispersant is sodium carboxymethyl cellulose; the ether cosolvent is propylene glycol ethyl ether;
the terpolymer is prepared from vinyl pyrrolidone, vinyl caprolactam and isopropyl-methacrylamide, and has an average molecular weight of 10000-18000 g/mol;
2. the preparation method of the hydrate inhibitor comprises the following steps:
(1) preparation of the terpolymer: according to a molar ratio of 1: 85: 10 adding three monomers of vinyl pyrrolidone, vinyl caprolactam and isopropyl-methacrylamide and an initiator into an alcohol solvent, and introducing N2After deoxidization, stirring and reacting for 16h at 40 ℃, cooling to room temperature, standing for 2h in a baking oven at 50 ℃, filtering, washing filter residues with water for 3 times, and drying in a vacuum drying oven to constant weight to obtain the terpolymer of vinyl pyrrolidone, vinyl caprolactam and isopropyl-methacrylamide; wherein the alcohol solvent is a mixed solution of propanol and n-butanol; the initiator is potassium persulfate; the volume ratio of the total volume of the three monomers to the alcohol solvent is 1: 4; the mass ratio of the total mass of the three monomers to the initiator is 1: 4;
(2) the terpolymer, the ether cosolvent and the dispersant are mixed and stirred.
3. Preparing the inhibitor into a gas field produced aqueous solution with the mass concentration of 1%, loading the aqueous solution into a reaction kettle, starting a test under the conditions that the test pressure is 7.0MPa and the test temperature is 3 ℃, and measuring the inhibition time of the generation of the natural gas hydrate to be 4250 min.
Example 3
1. A hydrate inhibitor comprises the following components in percentage by weight: 15% of terpolymer, 55% of ether cosolvent and 30% of dispersant;
wherein the dispersant is hydroxyethyl cellulose; the ether cosolvent is propylene glycol butyl ether;
the terpolymer is prepared from vinyl pyrrolidone, vinyl caprolactam and isopropyl-methacrylamide, and has an average molecular weight of 10000-18000 g/mol;
2. the preparation method of the hydrate inhibitor comprises the following steps:
(1) preparation of the terpolymer: according to a molar ratio of 25: 85: 10 adding three monomers of vinyl pyrrolidone, vinyl caprolactam and isopropyl-methacrylamide and an initiator into an alcohol solvent, and introducing N2After deoxidization, stirring and reacting for 5h at 85 ℃, cooling to room temperature, standing in a drying oven at 40 ℃ for 3h, filtering, washing filter residues with water for 3 times, and drying in a vacuum drying oven to constant weight to obtain the terpolymer of vinyl pyrrolidone, vinyl caprolactam and isopropyl-methacrylamide; wherein the alcohol solvent is a mixed solution of acetone and methanol; the initiator is hydrogen peroxide; the volume ratio of the total volume of the three monomers to the alcohol solvent is 1: 5; the mass ratio of the total mass of the three monomers to the initiator is 1: 5;
(2) the terpolymer, the ether cosolvent and the dispersant are mixed and stirred.
3. Preparing the inhibitor into a gas field produced aqueous solution with the mass concentration of 0.5%, loading the aqueous solution into a reaction kettle, starting a test under the conditions that the test pressure is 7.0MPa and the test temperature is 3 ℃, and measuring the inhibition time of the generation of the natural gas hydrate to be 4580 min.
Example 4
1. A hydrate inhibitor comprises the following components in percentage by weight: terpolymer 20%, ether cosolvent 55% and dispersant 25%;
wherein the dispersant is a mixture of methylcellulose, sodium carboxymethylcellulose and hydroxyethyl cellulose; the ether cosolvent is propylene glycol butyl ether;
the terpolymer was as in example 1.
2. The preparation method of the hydrate inhibitor is the same as that of example 1.
3. Preparing the inhibitor into a gas field produced aqueous solution with the mass concentration of 0.3%, loading the aqueous solution into a reaction kettle, starting a test under the conditions that the test pressure is 7.0MPa and the test temperature is 3 ℃, and measuring the inhibition time of the generation of the natural gas hydrate to be 4680 min.
Example 5
1. A hydrate inhibitor comprises the following components in percentage by weight: 15% of terpolymer, 70% of ether cosolvent and 15% of dispersant;
wherein the dispersant is a mixture of methylcellulose, sodium carboxymethylcellulose and hydroxyethyl cellulose; the ether cosolvent is propylene glycol butyl ether;
the terpolymer was as in example 2.
2. The preparation method of the hydrate inhibitor is the same as that of example 2.
3. Preparing the inhibitor into a gas field produced aqueous solution with the mass concentration of 0.3%, loading the aqueous solution into a reaction kettle, starting a test under the conditions that the test pressure is 7.0MPa and the test temperature is 3 ℃, and measuring the inhibition time of the generation of the natural gas hydrate to be 4720 min.
In examples 1 to 5, the dispersant was removed from the ingredients, and comparative examples 1 to 5 were disposed correspondingly, and the inhibition performance thereof was evaluated, and the results were as follows:
comparative example 1: 2450 min.
Comparative example 2: 2280 min.
Comparative example 3: 2540 min.
Comparative example 4: 2550 min.
Comparative example 5: 2590 min.
Meanwhile, a blank set was set as comparative example 6, thermodynamic inhibitor methanol as comparative example 7, and PVP as comparative example 8, respectively as follows:
comparative example 6
The produced water of the gas field with the mineralization degree of 52163mg/L is filled into a reaction kettle, the experiment is started under the conditions that the experiment pressure is 7.0MPa and the experiment temperature is 3 ℃, and the generation time of the natural gas hydrate is measured to be 40min by the method.
Comparative example 7
Preparing methanol into a gas field produced aqueous solution with the mass concentration of 40%, loading the aqueous solution into a reaction kettle, starting a test under the conditions that the test pressure is 7.0MPa and the test temperature is 3 ℃, and measuring the inhibition time of the generation of the natural gas hydrate to be 160 min.
Comparative example 8
PVP is prepared into a gas field produced aqueous solution with the mass concentration of 2%, the aqueous solution is placed into a reaction kettle, a test is started under the conditions that the test pressure is 7.0MPa and the test temperature is 3 ℃, and the inhibition time of the generation of the natural gas hydrate is 210 min.
Claims (7)
1. A hydrate inhibitor characterized by: the composite material comprises the following components in percentage by weight: 10-50% of terpolymer, 45-85% of ether cosolvent and 1-30% of dispersant;
wherein the terpolymer is a terpolymer of vinyl pyrrolidone, vinyl caprolactam and isopropyl methacrylamide;
the dispersant is at least one of methyl cellulose, sodium carboxymethyl cellulose and hydroxyethyl cellulose;
the ether cosolvent is any one of propylene glycol methyl ether, propylene glycol ethyl ether and propylene glycol butyl ether.
2. The hydrate inhibitor according to claim 1, wherein: the average molecular weight of the terpolymer was 10000-18000 g/mol.
3. A process for preparing the hydrate inhibitor according to claim 1, wherein: the method comprises the following steps:
(1) preparing a terpolymer;
(2) and then mixing and stirring the terpolymer, the ether cosolvent and the dispersant.
4. A process for preparing a hydrate inhibitor according to claim 3, wherein: the method for preparing the terpolymer in the step (1) is as follows: according to a molar ratio (1-25): (1-85): (1-10) adding three monomers of vinyl pyrrolidone, vinyl caprolactam and isopropyl-methacrylamide and an initiator into an alcohol solvent, and introducing N2After deoxidization, stirring and reacting for 5-16h at 40-85 ℃, cooling to room temperature, standing for 2-3h in an oven at 40-50 ℃, filtering, washing filter residues for 3 times by using water, and drying in a vacuum drying oven to constant weight to obtain the product; wherein, the volume ratio of the total volume of the three monomers to the alcohol solvent is 1: (3-5); the mass ratio of the total mass of the three monomers to the initiator is 1: (3-5).
5. The method for preparing the hydrate inhibitor according to claim 4, wherein: the alcohol solvent is at least two of acetone, methanol, ethanol, propanol, n-butanol and tert-butanol.
6. The method for preparing the hydrate inhibitor according to claim 4, wherein: the initiator is hydrogen peroxide, sodium persulfate, potassium persulfate or dimethyl azodiisobutyrate.
7. Use of the hydrate inhibitor according to claim 1, wherein: the application is as follows: adding the hydrate inhibitor into produced water of an oil-gas field according to the mass concentration of 0.1-1% under the pressure of 7.0MPa and at the temperature of 2-4 ℃.
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| CN113817443B (en) * | 2020-06-18 | 2022-08-30 | 中国石油化工股份有限公司 | Hydrate decomposition inhibiting composition, coupling enhanced solid hydrate and method for enhancing storage and transportation stability of solid hydrate |
| CN113214811B (en) * | 2021-04-09 | 2022-10-25 | 华南理工大学 | A high-efficiency low-dose compound inhibitor of natural gas hydrate and its application |
| CN114230716B (en) * | 2021-12-30 | 2022-08-05 | 清华大学深圳国际研究生院 | Preparation method and application of terpolymer |
| CN114316136B (en) * | 2022-01-13 | 2023-01-31 | 西华师范大学 | A kind of hydrogen bond enhanced hydrate inhibitor and preparation method thereof |
| CN116396429B (en) * | 2023-04-14 | 2023-10-13 | 西南石油大学 | A kind of natural gas hydrate kinetic inhibitor and preparation method thereof |
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