CN111548282A - Synthesis method and application of active supermolecule scale dissolver - Google Patents
Synthesis method and application of active supermolecule scale dissolver Download PDFInfo
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- CN111548282A CN111548282A CN202010496334.8A CN202010496334A CN111548282A CN 111548282 A CN111548282 A CN 111548282A CN 202010496334 A CN202010496334 A CN 202010496334A CN 111548282 A CN111548282 A CN 111548282A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
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- C—CHEMISTRY; METALLURGY
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- 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
- C09K8/528—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning inorganic depositions, e.g. sulfates or carbonates
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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
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/584—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific surfactants
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
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- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B37/00—Methods or apparatus for cleaning boreholes or wells
- E21B37/06—Methods or apparatus for cleaning boreholes or wells using chemical means for preventing, limiting or eliminating the deposition of paraffins or like substances
Abstract
The invention discloses a method for synthesizing an active supermolecule scale dissolver, which comprises the steps of adding organic amine, bihalogenated alkane, a phase transfer agent, a solvent and a pH regulator into a reaction vessel, wherein the molar ratio of the organic amine: bis-alkyl halides: phase transfer agent ═ (2.2-2.3): 1: (0.03-0.07); the mass ratio of the sum of the mass of the organic amine, the bihalogenated alkane and the phase transfer agent to the solvent is 1 (1-1.2); adding a pH regulator to regulate the pH value of the reaction system to 9-9.5; heating to 85-90 ℃, and stirring for reaction for 22-24 h to obtain the active supermolecule scale dissolver. The invention is suitable for dissolving and removing barium and strontium scales, water drive, gas drive, chemical drive injection and extraction layer barium and strontium scales and calcium carbonate scales of oil field gathering and transportation pipelines, improves the scale dissolving rate of insoluble scales such as the barium and strontium scales, reduces the corrosion of a general strong-alkaline scale dissolver to equipment, reduces the treatment cost of residual liquid and the damage to the environment, and improves the comprehensive benefit.
Description
Technical Field
The invention relates to the technical field of oil extraction and gas production engineering in the petroleum industry, in particular to a synthetic method of an active supermolecule scale dissolver and application thereof.
Background
The oil field development enters the middle and later stages, and the application of technologies such as water injection, tertiary oil recovery and the like causes the serious scaling problem of the oil field. The oilfield fouling type is carbonate scale (CaC 0)3) Sulfate scale (CaS 0)4、BaS04、SrS04) And iron scale, etc., and form mixed scales with each other. Scaling can occur in strata, mineshafts, equipment, ground systems and the like, so that oil gas pores and channels are blocked, the permeability is reduced, the oil gas yield is reduced, the energy consumption is increased, under-scale corrosion is generated, the normal production of an oil field is seriously influenced, the production efficiency is reduced, even a water injection well is scrapped, particularly, barium strontium scale is insoluble in acid, the texture is hard and difficult to remove, and great challenge is brought to later development of the oil field.
The main causes of barium sulfate scale formation are chemical incompatibility and thermodynamic instability. Chemical incompatibility is the leading cause of barium sulfate scale formation and when injected into water contains significant amounts of Ba2+Then, with the formation water S04 2+BaS0 is easily generated by meeting4And (4) scale formation. Since barium sulfate has a very low solubility product and produces a precipitate faster than other types of scales. The scale formation caused by thermodynamic instability is caused by the change of the influence factors such as temperature, pressure, pH, salt content and the like, and the original BaSO is broken4Dissolving equilibrium in water to cause precipitation of precipitate. The barium and strontium scale damage of the oil field is a problem faced by water flooding, gas flooding and chemical flooding of the oil field, and how to remove the formed barium and strontium scale is still one of the worldwide problems.
In the middle of the last 80 th century, the Dunlin and Brent oil fields in the sea area of the North sea of Shell Esso company firstly use EDTA (ethylene diamine tetraacetic acid) scale remover to carry out chemical removal operation of barium (strontium) sulfate scale in a well for more than 40 times in a squeezing mode, after closing the well for 24 hours, the production capacity of a few oil wells is slightly improved, but the scale remover achieves greater success on a well which is closed for 3 weeks, but when the EDTA is used for removing the barium sulfate scale, the scale remover cannot achieve the purpose of removing the scale within acceptable well closing time. However, recovery of production by re-perforation of partially barium (strontium) scale deposited wells has all been successful, only half of the wells can be recovered to pre-treatment levels. In addition, scale formation has never been found in the wellbore during workover operations, and sulfate in the injected water has been deposited in the pores of the formation as barium sulfate before reaching the bottom of the well. Under the condition of poor chemical descaling effect or high cost, Shell Esso company adopts a method of extruding and injecting a scale inhibitor into oriented stratum to control scaling, and the used scale inhibitor is mainly phosphate or a compound thereof, and the extrusion cycle is generally 4 months. The AKZO company uses AMAGARD 462 to chelate the scale remover, and the thermal cycle process removes the barium sulfate scale in the pipeline, the active ingredients of the scale remover decrease at a rate of about 1% per hour, and the removed scale contains 75% barium sulfate and 20% strontium sulfate.
The addition of the polymer barium sulfate and strontium scale inhibitor is 20mg/L-200mg/L, the scale prevention rate is more than 80% at the temperature of 70 ℃, but the polymer barium sulfate and strontium scale inhibitor has the defects of large dosage, scale prevention effect only on barium sulfate and strontium sulfate scales with low ion concentration, low scale prevention effect on barium sulfate and strontium sulfate scales with high ion concentration and poor scale dissolution performance on barium sulfate and strontium scales in actual use.
The domestic companies such as Heima successively develop composite complexing agents, barium and strontium scales are dissolved through complexing, the composite complexing agents and metal ions are mainly adopted to generate complexes, and a plurality of complexing rings are usually formed. The complex complexing agent can be simultaneously mixed with a plurality of metal ions such as Ca2+、Mg2+、Fe3+、Fe2+、Ba2+And Sr2+The plasma generates a complexing effect to generate a stable complex with higher solubility, prevents the particles from being combined with corresponding acid radicals and from generating precipitates, thereby effectively preventing secondary precipitates after the scale of the blocking remover is dissolved from blocking capillary and throat of oil field stratums. Complex complexing agentThe oxygen atoms in the polar groups of the molecules of the alkali have unshared electron pairs and can be used as adsorption centers to adsorb metal ions to form five-membered or six-membered cyclic compounds.
In 1978, the complete concept of "supramolecular chemistry" was first proposed by french scientist j.m. lelin (rayne), who pointed out that "supramolecular chemistry exists based on covalent bonds, and on molecular assemblies and molecular bonds". Supramolecular chemistry generally refers to the combination of two or more molecules, joined by intermolecular interactions, into complex, organized aggregates that retain some integrity, giving them a defined microstructure and macroscopic properties, the intermolecular relationships being the same as atoms forming molecules through covalent bonds. Molecular recognition is due to a specific, exclusive interaction between different molecules, which satisfies both the spatial requirements between the molecules that bind to each other and the matching of various secondary bonding forces between the molecules. In supramolecules, a particular portion of an acceptor molecule has certain groups, which are suitable for binding with groups of another substrate molecule, and when the acceptor molecule meets the substrate molecule, the acceptor molecule and the substrate molecule are mutually selected to form a secondary bond, or the acceptor molecule forms a structure suitable for a hole reserved by the substrate molecule through the secondary bond according to the size of the substrate molecule, so the essence of molecular recognition is the optimal condition for forming the secondary bond between the acceptor and the substrate molecule, and the two parties are mutually selected to be combined together, so that the system tends to be stable. The conventional scale dissolvers generally realize the scale dissolving effect through chelating reaction, but have limitations and unsatisfactory effect, and only can relieve the problem which cannot be solved fundamentally. When the molecular recognition and the chemical bond combination of the supermolecule scale dissolver are carried out, the original scale on the surface of equipment can be repelled and removed, and the cleaning function of thoroughly removing the scale is achieved.
At present, scale dissolution through a chelating reaction can only relieve scale formation, and a scale layer cannot be fundamentally removed. The pH value of the scale dissolving liquid prepared by dissolving barium and strontium scales by complex complexation is 11-13, the pH value is high, the residual liquid needs to be treated by acid liquor, and the treatment cost is high. Even some complex complexing agents have larger biological toxicity and cause damage to constructors and environment. The Bola type surfactant is different from the traditional surfactant consisting of a hydrophilic group and a hydrophobic chain, the special structure of the Bola type surfactant determines that the Bola type surfactant not only has the function of the traditional surfactant, but also has the capability of forming a stable monolayer lipid membrane and vesicle, unique surface performance and aggregation and self-assembly behaviors, when the Bola compound forms spherical micelles, the folding conformation can be adopted in the micelles, rod-shaped micelles can also be formed, a large number of cation and anion groups exist, the capabilities of complexing barium and strontium scales are realized, and no precipitate is generated due to the cation content, so that the application prospect of the amphiphilic Bola compound in the field of oil field scale prevention is displayed. The research and development of the supermolecule barium-strontium scale dissolver with high scale dissolving efficiency and environmental friendliness is the main direction of the technical development.
CN 105949395A discloses a molecular cluster material of supramolecular polymer and a preparation method thereof, which takes polystyrene microspheres as a substrate, and active groups containing a large amount of carboxyl or sulfonic groups are grafted on the surfaces of the polystyrene microspheres to synthesize the molecular cluster material. The preparation method is simple, low in cost, low in energy consumption, environment-friendly, pollution-free, efficient and stable in product, large in descaling amount and strong in oxidation resistance, but a multi-step synthesis process is adopted, and the requirements on synthesis conditions are strict.
Disclosure of Invention
The invention aims to provide an active supermolecule scale dissolver for barium and strontium scales, which improves the scale dissolving speed under a static condition, increases the scale dissolving rate, and solves the technical problems that a strong alkaline scale dissolver seriously corrodes equipment, has high acid-base neutralization cost for residual liquid treatment, has great environmental harm to heterocyclic complexing agents and the like.
The technical scheme provided by the invention is as follows:
a method for synthesizing an active supramolecular scale dissolver comprises the following steps:
adding an organic amine, a bis-haloalkane, a phase transfer agent, a solvent and a pH regulator into a reaction vessel, wherein the molar ratio of the organic amine: bis-alkyl halides: phase transfer agent ═ (2.2-2.3): 1: (0.03-0.07); the mass ratio of the sum of the mass of the organic amine, the bihalogenated alkane and the phase transfer agent to the solvent is 1 (1-1.2); adding a pH regulator to regulate the pH value of the reaction system to 9-9.5; heating to 85-90 ℃, and stirring for reaction for 22-24 h to obtain the active supermolecule scale dissolver.
Preferably, the organic amine includes sodium ethylenediaminetetraacetate, sodium diethylenetriaminepentaacetate, and heptasodium diethylenetriaminepentamethylenephosphonate.
Preferably, the bis-haloalkanes include 1, 6-dichlorohexane, 1, 8-dichlorooctane, 1, 10-dichlorodecane and 1, 10-dibromodecane.
Preferably, the phase transfer agent comprises tetrabutylammonium bromide, 12 alkyl dimethyl ammonium chloride and 12 alkyl dimethyl betaine.
Preferably, the pH adjusting agent comprises EDTA and Na2EDTA。
Preferably, the molar ratio of organic amine: bis-alkyl halides: phase transfer agent 2: 1: 0.05.
as another object of the present invention, the present invention also provides the active supramolecular detergent prepared by the above synthesis method.
As another object of the invention, the invention also provides the application of the supramolecular scale dissolver in descaling in oil field wellbores and perforations.
Preferably, preparing an active supermolecule scale dissolver aqueous solution with the mass concentration of 10-15%, injecting from the oil sleeve annulus, closing the well and extracting after 72 hours.
The invention has the beneficial effects that: the active supermolecule scale dissolver prepared by the invention is suitable for dissolving and removing barium and strontium scales of oil field gathering and transportation pipelines, water-driven, gas-driven and chemical-driven injection and extraction layers of barium and strontium scales, is suitable for dissolving and removing pollution blockage of barite slurry weighting agents, is also suitable for removing calcium carbonate scales, improves the scale dissolving rate of difficult scale dissolving such as barium and strontium scales, and the scale dissolving rate is more than 90%. Reduce the corrosion of the common strong alkaline detergent to equipment, reduce the treatment cost of residual liquid and the harm to the environment, and improve the comprehensive benefit.
Detailed Description
The technical solutions and advantages of the present invention will be explained and explained in more detail with reference to the detailed embodiments of the specification. It should be understood that the contents presented in the description and the detailed description are only for more clearly illustrating the technical solution and the advantages thereof, and do not limit the protection scope of the present invention. On the basis of the disclosure of the specification, a person skilled in the art can modify the technical solution according to various reasonable changes, and the modified technical solution is included in the protection scope of the invention as long as the person does not depart from the spirit of the invention.
A method for synthesizing an active supramolecular scale dissolver comprises the following steps:
adding an organic amine, a bis-haloalkane, a phase transfer agent, a solvent and a pH regulator into a reaction vessel, wherein the molar ratio of the organic amine: bis-alkyl halides: phase transfer agent ═ (2.2-2.3): 1: (0.03-0.07); the mass ratio of the sum of the mass of the organic amine, the bihalogenated alkane and the phase transfer agent to the solvent is 1 (1-1.2); adding a pH regulator to regulate the pH value of the reaction system to 9-9.5; heating to 85-90 ℃, and stirring for reaction for 22-24 h to obtain the active supermolecule scale dissolver.
The organic amine comprises sodium ethylene diamine tetracetate, sodium diethylenetriamine pentaacetate and heptasodium diethylenetriamine penta (methylene phosphonic acid).
The double halogenated alkyl comprises 1, 6-dichlorohexane, 1, 8-dichlorooctane, 1, 10-dichloro decane and 1, 10-dibromo decane.
The phase transfer agent includes tetrabutylammonium bromide, 12 alkyl dimethyl ammonium chloride and 12 alkyl dimethyl betaine.
The pH regulator comprises EDTA and Na2EDTA。
The reaction principle of the invention is as follows:
the synthetic product has the general formula
R1: at least 2 carboxylate or phosphate functions contained in the organic baseAnd (4) clustering.
X is chlorine atom or bromine atom.
n:3-12。
Example 1
Adding sodium ethylene diamine tetracetate, 1, 10-dichloro-decane, tetrabutylammonium bromide, water and a pH value regulator Na into a three-neck flask2EDTA, wherein the molar ratio of reactants, the phase transfer agent and the pH regulator is EDTA sodium: 1, 10-dichloro-decane: tetrabutylammonium bromide: na (Na)2EDTA ═ 2.2: 1: 0.05:0.08, heating to 87 ℃, and stirring for reaction for 22 hours to obtain the active supermolecular barium-strontium scale dissolver.
Example 2
Adding sodium diethylenetriamine pentaacetate, 1, 10-dibromodecane, 12-alkyl dimethyl betaine, water and a pH regulator EDTA into a three-neck flask, wherein the molar ratio of reactants, a phase transfer agent and the pH regulator is that of the sodium diethylenetriamine pentaacetate: 1, 10-dibromodecane: 12 alkyl dimethyl betaine: EDTA ═ 2.3: 1: 0.04:0.04, heating to 85-90 ℃, and stirring for reaction for 24 hours to obtain the active supermolecular barium-strontium scale dissolver.
Example 3
Testing the scale prevention performance of the active supermolecule scale inhibitor:
using the supramolecular scale solution of example 1, prepare a barium strontium scale solution: 12% by weight of the product of example 1 + 88% by weight of water, without any further additives being added to the formulation.
Preparing 100g of scale cleaning liquid according to a formula of the barium-strontium scale cleaning liquid, wherein the surface tension is 45mN/m at the temperature of 60 ℃; 50g of scale cleaning solution is taken, 1g of 100-mesh barium sulfate is added, and the mixture is kept stand in a constant temperature box at 60 ℃ for 72 hours, so that the scale dissolution rate is 90%.
Example 4
Testing the scale prevention performance of the active supermolecule scale inhibitor:
using the supramolecular scale solution of example 2, prepare a barium strontium scale solution: 12% by weight of the product of example 1 + 88% by weight of water, without any further additives being added to the formulation.
Preparing 100g of scale cleaning liquid according to a formula of the barium-strontium scale cleaning liquid, wherein the surface tension is 45mN/m at the temperature of 60 ℃; 50g of scale cleaning solution is taken, 1g of 100-mesh barium sulfate is added, and the mixture is kept stand in a constant temperature box at 60 ℃ for 72 hours, so that the scale dissolution rate is 92%.
Example 5
The production layer of the JS oilfield Y35 well is an E1f12 sandstone 6, 8 and 9 layers, the well section is (2103.6-2121.3) m, the effective thickness is 8.9m, the porosity is 12.3%, the permeability is 12.4 × 10-3 μm2, the JS oil field belongs to a low-pore-extra-low-permeability reservoir, the stratum temperature is 79 ℃, and the yield is obviously reduced due to barium strontium scale of a shaft and a perforation hole3The scale dissolving liquid is injected from the oil sleeve annulus, pumping is carried out after the well is closed for 72 hours, the daily oil yield after scale dissolving is increased from 1.5t/d before scale dissolving to 3.4t/d, and the oil increasing effect is obvious.
Claims (10)
1. A method for synthesizing an active supramolecular scale dissolver is characterized by comprising the following steps:
adding an organic amine, a bis-haloalkane, a phase transfer agent, a solvent and a pH regulator into a reaction vessel, wherein the molar ratio of the organic amine: bis-alkyl halides: phase transfer agent ═ (2.2-2.3): 1: (0.03-0.07); the mass ratio of the sum of the mass of the organic amine, the bihalogenated alkane and the phase transfer agent to the solvent is 1 (1-1.2); adding a pH regulator to regulate the pH value of the reaction system to 9-9.5; heating to 85-90 ℃, and stirring for reaction for 22-24 h to obtain the active supermolecule scale dissolver.
2. The method of synthesis of claim 1, wherein the organic amine comprises sodium ethylenediaminetetraacetate, sodium diethylenetriaminepentaacetate, and heptasodium diethylenetriaminepentamethylenephosphonic acid.
3. The method of claim 1, wherein the bis-haloalkanes comprise 1, 6-dichlorohexane, 1, 8-dichlorooctane, 1, 10-dichlorodecane, and 1, 10-dibromodecane.
4. The synthetic method of claim 1 wherein the phase transfer agent comprises tetrabutylammonium bromide, 12 alkyl dimethyl ammonium chloride and 12 alkyl dimethyl betaine.
5. The method of synthesis of claims 1-4, wherein the pH adjusting agent comprises EDTA and Na2EDTA。
6. The synthesis method according to claim 1, wherein the molar ratio of the organic amine: bis-alkyl halides: phase transfer agent 2: 1: 0.05.
7. active supramolecular detergent prepared by the synthesis method of any one of claims 1-6.
8. Use of the reactive supramolecular detergent of claim 6 for descaling in oil field wellbores and perforations.
9. The use of claim 8, wherein the active supramolecular scale dissolver aqueous solution with the mass concentration of 10-15% is prepared, injected from the oil casing annulus, and extracted after the well is closed for 72 hours.
10. Use according to claim 9, characterized in that the concentration of the aqueous solution of active supramolecular detergent is 12 wt%.
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| CN114426823A (en) * | 2021-12-30 | 2022-05-03 | 中国石油化工股份有限公司 | Oil field insoluble scale dispersing solubilizer and preparation method thereof |
| CN114517661A (en) * | 2020-11-20 | 2022-05-20 | 中国石油天然气股份有限公司 | Method for determining water injection block descaling measures |
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