CN113072922B - Magnetic hydrate inhibitor, slurry and preparation method thereof - Google Patents
Magnetic hydrate inhibitor, slurry and preparation method thereof Download PDFInfo
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- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
- C09K8/524—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning organic depositions, e.g. paraffins or asphaltenes
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Abstract
The invention discloses a magnetic hydrate inhibitor, slurry and a preparation method thereof, wherein the method comprises the following steps: 1) preparing spherical magnetic nanoparticles; 2) coating the spherical magnetic nanoparticles in 1) with silicon dioxide. 3) Modifying the functional groups of the magnetic particles coated with the silicon dioxide in the step 2). 4) Carrying out inhibitor loading on the modified magnetic particles in the step 3). 5) And (4) carrying out solvent dispersion on the magnetic particles loaded with the inhibitor in the step 4) to prepare hydrate inhibitor slurry. In the hydrate inhibitor slurry, the nano particles have good dispersibility, have the hydrate inhibition function and can be separated and recovered under the action of a magnetic field. The invention has the advantages that the using amount of the traditional inhibitor can be effectively saved, and the simple modularization of the preparation process has potential wide application in inhibitor using schemes.
Description
Technical Field
The invention relates to the technical field of oil and gas industry, in particular to a recyclable magnetic hydrate inhibitor, recyclable magnetic hydrate slurry and a preparation method of the recyclable magnetic hydrate inhibitor and the recyclable magnetic hydrate slurry.
Background
Natural gas hydrate is a crystalline solid similar to ice, and is a cage-like molecule formed by interaction of gases under high pressure and low temperature conditions. Typical gas molecules involved in natural gas hydrate formation include light hydrocarbons such as methane, ethane, propane and isobutane, as well as gases such as hydrogen sulfide and carbon dioxide. The pipeline blockage of the natural gas hydrate is a main flow guarantee problem in the petroleum industry, and is particularly common in multiphase flow pipelines under seabed and cold climate conditions, and CN201610644140.1 is a composite inhibitor of the natural gas hydrate and application thereof.
One method of controlling hydrate blockage is the synthesis of polyvinyl caprolactam, the hydrate kinetic inhibitor, CN201210184096.2 hydrate inhibitor, which is a low dosage inhibitor compared to conventional thermodynamic inhibitors, and which is generally based on water-soluble polymers, usually containing amide or imide functionality, and can be applied at lower concentrations, and which is generally applied in an amount of between 0.5% wt and 2% wt depending on the amount of water produced on site.
In the production process of oil and gas fields, the added thermodynamic inhibitor and kinetic inhibitor often have the defects of large injection amount, high cost, high toxicity and the like, and CN202010962286.7 is a magnetic targeted hydrate inhibitor transportation system and method. At present, the research direction for hydrate inhibitors at home and abroad mainly tends to develop low-dosage hydrate inhibitors such as kinetic inhibitors, anti-agglomerants and the like so as to reduce the dosage of the inhibitors and further reduce the production cost, but the method still has great promotion space for the whole large oil and gas production, storage and transportation pipeline. Therefore, the development of a novel low-cost magnetic recoverable inhibitor has important significance for preventing hydrate from blocking an oil and gas transportation pipeline and further reducing the exploitation cost.
Disclosure of Invention
Aiming at the technical defects of the prior art, the invention provides a recyclable magnetic hydrate inhibitor slurry and a preparation method thereof, wherein the magnetic hydrate inhibitor can effectively inhibit the growth of natural gas hydrates in the gas field exploitation and transportation processes, and can be effectively recycled under the condition of a magnetic field.
The preparation method of the magnetic hydrate inhibitor provided by the invention comprises the following steps:
step 1, coating a magnetic nanoparticle core with silicon dioxide; the magnetic nano particle core comprises at least one of cobaltosic oxide and ferroferric oxide;
and 3, loading the inhibitor after modification in the step 2, wherein the adopted inhibitor raw material is a polymer or copolymer formed by polymerizing one or a mixture of more than two of vinyl caprolactam, vinyl pyrrolidone, vinyl valerolactam, vinyl heptanolactam and isopropyl acrylamide.
Preferably, the method for preparing the magnetic nanoparticle core in step 1) is specifically as follows: according to a molar ratio (1-20): (1-50): 1: (1-20) adding polyoxyethylene alkylolamide, an alcohol solvent, ferric trichloride and sodium chloride into a beaker, stirring and dissolving, introducing nitrogen to remove oxygen, transferring into a hydrothermal kettle, reacting at 100-200 ℃ for 24-48h, cooling to room temperature, washing with water and ethanol respectively, and drying in a vacuum drying oven. According to the weight ratio (1-60): (1-200): (1-50): (1-20): 1 adding the magnetic nanoparticle core, ethanol, water, ammonia water and tetraethyl orthosilicate into a beaker, stirring, uniformly dispersing by ultrasonic wave, stirring at 25-50 ℃ for 10-24h, washing with water and ethanol respectively, and drying in a vacuum drying oven.
Preferably, the method for modifying the functional groups of the silica-coated magnetic nanoparticles in step 2) is as follows: according to the weight ratio (1-200): 1: (1-10) adding toluene, the magnetic nano-particles coated with the silicon dioxide prepared in the step 2) and a silane coupling agent into a beaker, stirring for 15min, performing ultrasonic treatment for 30min to uniformly disperse, stirring for 10-24h at 20-90 ℃, washing with water and ethanol respectively, and drying in a vacuum drying oven. Wherein the silane coupling agent is at least one of octyl trimethoxy silane, propenyl trimethoxy silane, chloromethyl trimethoxy silane, 3-aminopropyl trimethoxy silane, (3-acetamidopropyl) trimethoxy silane and (3-methoxypropyl) trimethoxy silane.
Preferably, the method for polymerizing the graft loading inhibitor on the nanoparticles in the step 3) is as follows: according to the weight ratio of 1: (1-60): (1-10): (1-200) adding the modified magnetic nano-particles coated by the silicon dioxide, the high molecular monomer, the initiator and the isopropanol prepared in the step 3) into a beaker, stirring for 15min, introducing nitrogen to remove oxygen, reacting for nitrogen protection, stirring for 5-24h at 20-120 ℃, performing rotary evaporation to remove the solvent, and then adding tetrahydrofuran and n-hexane, wherein the weight ratio of the tetrahydrofuran to the n-hexane to the modified magnetic nano-particles coated by the silicon dioxide is 1-100: 1-100: 1, separating precipitate, filtering, and drying in a vacuum drying oven to obtain the final magnetic hydrate inhibitor.
The high-molecular monomer is one or a mixture of more than two of vinyl caprolactam, vinyl pyrrolidone, vinyl valerolactam, vinyl heptanolactam and isopropyl acrylamide, and the initiator is at least one of potassium persulfate, azobisisobutyronitrile, benzoyl peroxide and hydrogen peroxide.
The magnetic hydrate inhibitor slurry comprises the following components in parts by weight: 1-10 parts of water, 10-80 parts of alcohol dispersant, 1 part of magnetic hydrate inhibitor and 1-10 parts of synergist.
The magnetic hydrate inhibitor slurry can also comprise the following components in parts by weight: 1-5 parts of water, 10-100 parts of alcohol dispersant and 1 part of magnetic nano-particles.
Wherein the synergist is at least one of ethylene glycol monopropyl ether, tetrabutylammonium bromide, tetra-n-hexyltrimethylammonium bromide and tetra-heptyltrimethylammonium bromide.
Wherein the alcohol dispersant is at least one of methanol, ethylene glycol, glycerol and isopropanol.
The preparation process of the magnetic hydrate inhibitor slurry comprises the following steps:
1) taking water, an alcohol dispersant and a synergist in a formula amount, and uniformly stirring at 300 revolutions per minute;
2) adding the magnetic nano particles 200 and 350 revolutions per minute in the formula amount and uniformly stirring.
The invention has the beneficial effects that:
according to the hydrate inhibitor slurry provided by the invention, the magnetic nanoparticles load the kinetic inhibitor, and the cosolvent and the synergist in the slurry are added, so that the inhibiting effect on the generation of the hydrate can be enhanced in the using process, and meanwhile, the magnetic particles can be rapidly separated and recovered under the magnetic field condition. The natural gas hydrate inhibitor can be used for inhibiting the generation of the natural gas hydrate in the processes of exploitation, treatment and transportation of an oil and gas field, has an obvious inhibiting effect, can be recovered, reduces the use cost, and is environment-friendly.
Drawings
FIG. 1 is a scanning electron micrograph of magnetic nanoparticles obtained in the present invention;
FIG. 2 is a temperature-pressure change curve of pure water in the comparative example;
FIG. 3 is a graph showing the temperature and pressure change after the magnetic slurry was added in the comparative example.
Detailed Description
In order to explain the technical content and the scheme of the embodiment of the invention, the embodiment is described below with the accompanying drawings.
Example 1
1. The magnetic hydrate inhibition slurry comprises the following components in percentage by weight: 5% of water, 60% of alcohol dispersant and 10% of magnetic nanoparticles;
wherein the alcohol dispersant is methanol, and the synergist is ethylene glycol monopropyl ether;
2. the preparation method of the magnetic nano-particles comprises the following steps:
(1) preparing a magnetic nanoparticle core: according to a molar ratio of 5: 1: 7: 15 adding polyoxyethylene alkylolamide, an alcohol solvent, ferric trichloride and sodium chloride into a beaker, stirring and dissolving, introducing nitrogen to remove oxygen, transferring into a hydrothermal kettle, reacting for 24 hours at 120 ℃, cooling to room temperature, washing with water and ethanol respectively, and drying in a vacuum drying oven.
(2) Coating silicon dioxide: according to the weight ratio of 5: 70: 20: 10: 1 adding the magnetic nanoparticle core, ethanol, water, ammonia water and tetraethyl orthosilicate into a beaker, stirring for 10min, performing ultrasonic treatment for 30min to disperse uniformly, stirring for 24h at 50 ℃, washing with water and ethanol respectively, and drying in a vacuum drying oven.
(3) Modifying the magnetic nano-particles coated with the silicon dioxide by functional groups: according to the weight ratio of 100: 10: 1 adding toluene, the prepared magnetic nano-particles coated by the silicon dioxide and a silane coupling agent into a beaker, stirring for 15min, performing ultrasonic treatment for 30min to disperse uniformly, stirring for 24h at 70 ℃, washing with water and ethanol respectively, and drying in a vacuum drying oven. Wherein the silane coupling agent is octyl trimethoxy silane.
(4) Subjecting the nanoparticles to polymerization graft loading inhibitor: according to the weight ratio of 1: 50: 5: 50 adding the modified magnetic nano-particles coated by the silicon dioxide, the high molecular monomer, the initiator and the isopropanol into a beaker, stirring for 15min, introducing nitrogen to remove oxygen, reacting for nitrogen protection, stirring for 10h at 100 ℃, carrying out rotary evaporation to remove the solvent, adding 10 weight parts of tetrahydrofuran and 10 weight parts of n-hexane for precipitation separation, filtering, and drying in a vacuum drying oven. Wherein the high molecular monomer is ethylene valerolactam and ethylene enantholactam. The initiator is benzoyl peroxide.
3. The preparation method of the magnetic hydrate inhibitor slurry comprises the following steps:
1) 5 percent of water and 60 percent of alcohol dispersant are evenly stirred at the speed of 100-; wherein the alcohol dispersant is methanol;
2) 10 percent of magnetic nano particles with the formula amount are added and stirred evenly at 200-350 r/min.
Example 2
1. The magnetic hydrate inhibition slurry comprises the following components in percentage by weight: 2% of water, 40% of alcohol dispersant, 10% of magnetic nanoparticles and 5% of synergist;
wherein the alcohol dispersant is ethylene glycol, and the synergist is tetrabutylammonium bromide;
2. the preparation method of the magnetic nano-particles comprises the following steps:
(1) preparing a magnetic nanoparticle core: according to a molar ratio of 7: 1: 10: 20 adding polyoxyethylene alkylolamide, an alcohol solvent, ferric trichloride and sodium chloride into a beaker, stirring and dissolving, introducing nitrogen to remove oxygen, transferring into a hydrothermal kettle, reacting for 24 hours at 120 ℃, cooling to room temperature, washing with water and ethanol respectively, and drying in a vacuum drying oven.
(2) Coating silicon dioxide: according to the weight ratio of 2: 50: 15: 5: 1 adding the magnetic nanoparticle core, ethanol, water, ammonia water and tetraethyl orthosilicate into a beaker, stirring for 10min, performing ultrasonic treatment for 30min to disperse uniformly, stirring for 12h at 25 ℃, washing with water and ethanol respectively, and drying in a vacuum drying oven.
(3) Modifying the magnetic nano-particles coated with the silicon dioxide by functional groups: according to the weight ratio of 50: 5: 1 adding toluene, the prepared magnetic nano-particles coated by the silicon dioxide and a silane coupling agent into a beaker, stirring for 15min, performing ultrasonic treatment for 30min to disperse uniformly, stirring for 12h at 50 ℃, washing with water and ethanol respectively, and drying in a vacuum drying oven. Wherein the silane coupling agent is octyl trimethoxy silane.
(4) Subjecting the nanoparticles to polymerization graft loading inhibitor: according to the weight ratio of 1: 20: 2: 90 adding the modified magnetic nano-particles coated by the silicon dioxide, the high molecular monomer, the initiator and the isopropanol into a beaker, stirring for 15min, introducing nitrogen to remove oxygen, reacting for nitrogen protection, stirring for 24h at 110 ℃, carrying out rotary evaporation to remove the solvent, adding tetrahydrofuran and n-hexane 20 in a molar ratio of 1, precipitating, separating, filtering, and drying in a vacuum drying oven. Wherein the high molecular monomer is vinyl caprolactam and vinyl pyrrolidone. The initiator is potassium persulfate.
3. The preparation method of the magnetic hydrate inhibitor slurry comprises the following steps:
1) taking 3% of water, 50% of alcohol dispersant and 10% of synergist, and uniformly stirring at the speed of 100-; wherein the alcohol dispersant is methanol, and the synergist is ethylene glycol monopropyl ether;
2) adding 5% of magnetic nano particles according to the formula amount, and uniformly stirring at 200-350 r/min.
Comparative example
1. Dispersing the magnetic inhibitor slurry in water by weight ratio of 10% and adding into an autoclave, controlling the temperature at 10 ℃, then flushing 7Mpa methane gas, controlling the temperature to uniformly reduce to 1 ℃ within 400min and keeping. The hydrate formation process was monitored by temperature and pressure sensors inside the autoclave.
2. Adding the same weight of the water-nondispersive magnetic inhibitor slurry into an autoclave, controlling the temperature to be 10 ℃, then flushing 7Mpa methane gas, controlling the temperature to be uniformly reduced to 1 ℃ within 400min, and keeping the temperature. The hydrate formation process was monitored by temperature and pressure sensors inside the autoclave.
3. The system added with the magnetic inhibitor slurry can be judged to have obvious inhibition performance on the generation of the hydrate through a temperature pressure change curve, and the generation induction time of the hydrate is increased by 950 min.
Claims (7)
1. A preparation method of a magnetic hydrate inhibitor is characterized in that modification and inhibitor loading are carried out after magnetic particles are coated by silicon dioxide, and comprises the following steps:
step 1, coating a magnetic nanoparticle core with silicon dioxide; the magnetic nano particle core comprises at least one of cobaltosic oxide and ferroferric oxide;
step 2, performing functional group modification after the silicon dioxide coating in the step 1, wherein the used silane coupling agent is at least one of octyl trimethoxy silane, propenyl trimethoxy silane, chloromethyl trimethoxy silane, 3-aminopropyl trimethoxy silane, (3-acetamidopropyl) trimethoxy silane and (3-methoxypropyl) trimethoxy silane;
step 3, loading the inhibitor after modification in the step 2, wherein the adopted inhibitor raw material is a polymer formed by polymerization of one or a mixture of more than two of vinyl caprolactam, vinyl pyrrolidone, vinyl valerolactam, vinyl heptanolactam and isopropyl acrylamide; the method for polymerizing and grafting the load inhibitor on the modified magnetic nanoparticles comprises the following specific steps: according to the weight ratio of 1: (1-60): (1-10): (1-200) adding the modified magnetic nano-particles coated by the silicon dioxide prepared in the step (2), a high-molecular monomer, an initiator and isopropanol into a beaker, and stirring, wherein the initiator is at least one of potassium persulfate, azodiisobutyronitrile, benzoyl peroxide and hydrogen peroxide; introducing nitrogen to remove oxygen, reacting for nitrogen protection, stirring for 5-24h at 20-120 ℃, performing rotary evaporation to remove a solvent, and then adding tetrahydrofuran and n-hexane, wherein the weight ratio of the tetrahydrofuran to the n-hexane to the modified magnetic nano-particles coated by the silicon dioxide is 1-100: 1-100: 1, separating precipitate, filtering, and drying in a vacuum drying oven to obtain the final magnetic hydrate inhibitor.
2. The method for preparing a magnetic hydrate inhibitor according to claim 1, wherein the method for preparing the magnetic nanoparticle core in the step 1 specifically comprises the following steps: according to a molar ratio (1-20): (1-50): 1: (1-20) adding polyoxyethylene alkylolamide, an alcohol solvent, a metal chloride salt and sodium chloride into a beaker, stirring and dissolving, wherein the alcohol solvent is one of ethylene glycol, glycerol and mannitol, the metal chloride salt is one of ferric chloride and cobalt chloride, introducing nitrogen to remove oxygen, transferring the mixture into a hydrothermal kettle, reacting for 24-48h at 100-200 ℃, cooling to room temperature, washing with water and ethanol respectively, and drying in a vacuum drying oven to obtain the magnetic nanoparticle core.
3. The method for preparing the magnetic hydrate inhibitor according to claim 1, wherein the method for coating the silica in the step 2 specifically comprises the following steps: according to the weight ratio (1-60): (1-200): (1-50): (1-20): 1, adding the magnetic nanoparticle core, ethanol, water, ammonia water and tetraethyl orthosilicate into a beaker, stirring, ultrasonically dispersing uniformly, stirring for 10-24h at 25-50 ℃, washing with water and ethanol respectively, and drying in a vacuum drying oven to obtain the magnetic nanoparticle coated with silicon dioxide.
4. The method for preparing a magnetic hydrate inhibitor according to claim 1, wherein the method for modifying the functional groups of the silica-coated magnetic nanoparticles in the step 2 is as follows: according to the weight ratio (1-200): 1: (1-10) adding toluene, magnetic nano-particles coated by silicon dioxide and a silane coupling agent into a beaker, stirring, ultrasonically dispersing uniformly, stirring for 10-24h at 20-90 ℃, washing with water and ethanol respectively, and drying in a vacuum drying oven to obtain the modified magnetic nano-particles.
5. The slurry for synthesizing the magnetic hydrate inhibitor, which is prepared by the method of any one of claims 1 to 4, is characterized by comprising the following components in parts by weight: 1-10 parts of water, 10-80 parts of alcohol dispersant, 1 part of magnetic hydrate inhibitor and 1-10 parts of synergist.
6. The slurry of claim 5, wherein the alcohol dispersant is one of methanol, ethylene glycol, glycerol, and isopropanol.
7. The slurry according to claim 6, wherein the synergist is selected from at least one of ethylene glycol monopropyl ether, tetrabutyl ammonium bromide, tetra-n-hexyl trimethyl ammonium bromide, tetra-heptyl trimethyl ammonium bromide.
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