CN111621278A - Synthesis method and application of macrocyclic compound supermolecule scale-dissolving material - Google Patents
Synthesis method and application of macrocyclic compound supermolecule scale-dissolving material Download PDFInfo
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Abstract
The invention discloses a synthesis method of a macrocyclic compound supermolecule scale-dissolving material, which comprises the following steps: preparing a supramolecular inclusion body; and (II) compounding the supermolecule antiscaling agent. The supermolecule composite material is formed by a host-guest synthesized inclusion body, and meanwhile, the scale inhibitor is formed by adding the auxiliary agents such as the solubilizer, the complexing agent and the like, can be applied to the field of scale prevention and control of oil and gas fields and other industries in the petroleum industry, is particularly suitable for preventing and controlling barium and strontium scales, has the pH value of about 9, is environment-friendly, and improves the scale prevention efficiency and the scale prevention effect.
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 synthesis method and application of a macrocyclic compound supermolecule scale-dissolving material.
Background
The water content continuously rises as the development of the oil field continuously enters the middle and later stages, a large amount of barium and strontium ions in the water of the oil field easily generate barium sulfate and strontium sulfate scales, and the scales can be formed 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 the oil field is seriously influenced, the production efficiency is reduced, even a water injection well is scrapped, particularly, the barium and strontium scales are insoluble in acid, the texture is hard, the removal is difficult, and great challenges are brought to the later-stage development of.
When injected into water, contains a large amount of Ba2+While, with the SO in the formation water4 2+BaSO is easily generated when 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 common problem in water flooding, gas flooding and chemical flooding of the oil field, and how to prevent and control the barium and strontium scale is still one of the worldwide problems.
The copolymer antiscaling agent has the advantages of excellent performance, good thermal stability, capability of synergistic action with organic phosphonate, and the like, has good complexing effect on barium ions and strontium ions, and is a research hotspot of water treatment agents. The anti-scaling agent mainly plays a role in scale prevention through chelation and adsorption. Scale inhibitor with chelating ability Ba2+And Sr2+Chelating to make it unable to react with SO4 2+Barium sulfate and strontium scale are generated by reaction. In the molecular design of the polymer chelating agent, the polymer chelating agent is considered to have groups with strong chelating ability as much as possible, so that the aim of better scale prevention is fulfilled.
The carboxylic acid group-containing polymer has a great amount of carboxylic acid groups in molecular chains, so that the chelating effect and the lattice distortion effect on barium ions and strontium ions in water can be realized; increasing the water solubility of the molecule increases the saturated solubility of the sparingly soluble salt in water. However, a polymer having only a carboxyl group in the molecule is likely to form a gel in a high-salt aqueous solution, and when a hydroxyl group, an amide group or a sulfonic acid group is introduced into the molecule, the solubility of the scale inhibitor can be improved to prevent the formation of a gel. Common carboxylic acid group-containing monomers are acrylic acid, maleic anhydride, and the like.
The sulfonic acid group is a strong polar group, has strong water solubility and is easy to dissolve in a polar solvent. The two O bonds and 3 strongly electronegative oxygens on this group share a negative charge, making them insensitive to attack by external cations. The molecules of the antiscaling agent contain a large amount of carboxylic acid groups and a certain proportion of sulfonic acid groups, so that the temperature resistance and salt resistance of the antiscaling agent can be improved, and the application range of the antiscaling agent of carboxylic acid polymer is expanded. A common monomer is sodium allylsulfonate.
A phosphorus-containing group having an excellent chelating ability for barium and strontium ions. This group is typically obtained by reaction with sodium hypophosphite.
The lipid group is an active group which can prevent polymer gel, has higher electron density and better adsorption effect, and changes the growth process of crystals by adsorbing generated crystal grains.
The copolymer antiscaling agent is the focus of main research at home and abroad, and presents a large number of antiscaling agent products represented by polyacrylamide and polymaleic acid-acrylic acid, the addition amount of the polymer barium sulfate and strontium antiscaling agent is 20mg/L-200mg/L, the antiscaling rate is more than 80% at the temperature of more than 70 ℃, but the copolymer antiscaling agent has the defects of large dosage, antiscaling effect only on barium sulfate and sulfuric acid with low ion concentration, and low antiscaling effect on barium sulfate and sulfuric acid with high ion concentration in practical use.
The conventional scale inhibitor generally realizes scale prevention through chelating reaction, not only has poor effect, but also cannot fundamentally solve the scale prevention problem. In recent years, the technology of the supramolecular material is rapidly developed, a network structure supramolecular antiscale material containing a large amount of chelating groups can be formed by utilizing the recognition and self-assembly functions of supramolecular molecules so as to improve the chelating capacity, and the network structure can change the crystal growth process; the supermolecule scale inhibitor can repel the original scale layer on the surface of equipment by utilizing the functions of supermolecule molecule recognition and chemical bonds, has the scale cleaning function, shows the application prospect of the supermolecule material in the field of oil field scale prevention, researches and develops the supermolecule scale inhibitor product, replaces the existing scale inhibitor in the field of oil extraction and gas production engineering, particularly improves the scale prevention efficiency, increases the scale cleaning function and improves the technical application effect in the technical field of oil and gas field barium and strontium scale prevention.
CN106186372A discloses a supramolecular care agent, which comprises the following components in percentage by weight: sodium alkyl benzene sulfonate, sodium polyacrylate, dodecyl dimethyl benzyl ammonium chloride, fatty alcohol-polyoxyethylene ether, etc. The nursing agent forms supermolecules based on the compounding of cations and anions, and simultaneously adds a nonionic surfactant and a mutual solvent, thereby having good control effect on industrial circulating water scaling, particularly carbonate scaling. However, the pH value of the nursing agent is high and reaches 10-10.5, the treatment cost of the residual liquid is high, the used components are multiple, and the product quality control is difficult.
CN 103007768A discloses a composite scale inhibitor for a reverse osmosis/nanofiltration system, which obtains better synergistic effect by mixing amino trimethylene phosphonic acid ATMP, hydroxyethylidene diphosphonic acid HEDP, 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid PBTCA, maleic anhydride-acrylic acid copolymer MA-AA and 2, 2-dibromo-3-cyano propionamide DBNPA in different proportions, and has excellent chelating solubilization, lattice distortion and coagulation dispersion effects on inorganic scale forming ions and inorganic scales. However, the scale inhibitor mainly aims at reverse osmosis membranes and nanofiltration membrane systems, and is not suitable for large-scale oil field scale removal operation.
Disclosure of Invention
The invention aims to provide a macrocyclic compound supermolecule antiscaling agent which replaces the original barium-strontium scale antiscaling agent in the oil extraction and gas production engineering fields, improves the antiscaling efficiency and improves the antiscaling effect.
The technical scheme provided by the invention is as follows:
a synthesis method of macrocyclic compound supermolecule scale-dissolving material comprises the following steps:
preparation of supramolecular inclusion body
Adding a component A, a component B, a component C and water into a reaction container, wherein the molar ratio of the component A to the component B is 1: (1-1.3), the mass ratio of the (component A + the component B), the component C and the water is (38-42) to (4-6) to (40-48), stirring and heating to (60-70) DEG C, and reacting for (2-3) h to obtain a mixture containing a supramolecular inclusion body;
the component A is a macrocyclic compound, including beta cyclodextrin, gamma cyclodextrin, 18-crown-6 ether, calix [6] arene and calix [8] arene;
b is selected from quaternary ammonium salt cationic surfactants and zwitterionic surfactants with 12-18 carbon atoms and a hydrophobic tail chain.
Component C is selected from low molecular weight alcohols, such as ethylene glycol, n-butanol and/or 1,2 propylene glycol;
(II) compounding of supermolecule antiscaling agent
Continuously adding 4-6.5 wt% of solubilizer, 2-3 wt% of complexing agent and 2-3 wt% of stripping agent, and stirring at normal temperature for 2-3h to obtain the compound supramolecular scale inhibitor.
Preferably, the solubilizer is a halogen salt, further comprising potassium chloride, sodium chloride, potassium bromide and/or sodium bromide.
Preferably, the complexing agent comprises an aminocarboxylate, a hydroxycarboxylic acid salt, an organic phosphonate, a polyacrylic acid, a phosphate, an alcohol amine and/or sodium gluconate.
Preferably, the stripping agent is a cationic surfactant containing large pi bonds, and further comprises alkyl phenyl dimethyl ammonium chloride with 8-18 carbon atoms and brominated alkyl pyridine with 8-18 carbon atoms.
Preferably, in step (one), the molar ratio of component A to component B is 1: 1.1.
preferably, in step (one), the mass ratio of (component a + component B), component C and water is 40:5: 45.
Preferably, in the step (two), the mass ratio of the solubilizer to the complexing agent to the stripping agent is 2:1: 1.
As another object of the present invention, the present invention also provides a supramolecular scale inhibitor prepared by the above synthesis method.
As another object of the invention, the invention also provides the use of the supramolecular scale inhibitor for descaling in oil field gathering pipelines.
Preferably, the scale inhibitor is added in the gathering pipeline at 25mg/l and 60 ℃.
As another object of the invention, the invention also provides the application of the supramolecular scale inhibitor in descaling in oil field wellbores and perforations.
Preferably, a supermolecule antiscalant aqueous solution with the mass fraction of 12% is prepared for 30m3Injecting from the oil casing annulus, closing the well and pumping out after 72 hours.
The invention has the beneficial effects that: the active supermolecule scale dissolver prepared by the invention can replace the existing barium and strontium scale dissolver in the field of oil extraction engineering, and the supermolecule scale dissolver can quickly diffuse to the surface of the barium and strontium scale by utilizing the surface activity of the supermolecule scale dissolver, so that the scale dissolving speed under a static condition is improved; the scale dissolving rate is increased by utilizing the molecular self-assembly and molecular recognition of the supermolecule scale dissolver and the super strong charge repulsion effect on the barium and strontium scales, and can reach more than 90 percent at most. Meanwhile, the technical problems that the strong-alkaline scale dissolver seriously corrodes equipment, the residual liquid treatment is high in acid-base neutralization cost, the heterocyclic complexing agent is greatly harmful to the environment and the like are solved.
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 synthesis method of macrocyclic compound supermolecule scale-dissolving material comprises the following steps:
preparation of supramolecular inclusion body
Adding a component A, a component B, a component C and water into a reaction container, wherein the molar ratio of the component A to the component B is 1: (1-1.3), the mass ratio of the (component A + the component B), the component C and the water is (38-42) to (4-6) to (40-48), stirring and heating to (60-70) DEG C, and reacting for (2-3) h to obtain a mixture containing a supramolecular inclusion body;
the component A is a macrocyclic compound, including beta cyclodextrin, gamma cyclodextrin, 18-crown-6 ether, calix [6] arene and calix [8] arene;
component B is selected from quaternary ammonium salt cationic surfactants and zwitterionic surfactants with 12-18 carbon atoms and a hydrophobic tail chain.
Component C is selected from low molecular weight alcohols, such as ethylene glycol, n-butanol and/or 1,2 propylene glycol;
the reaction principle of this step is schematically shown in equation:
a: represents component A;
b: represents component B;
c: represents a supramolecular inclusion body;
x: represents the hydrophilic group in component A
Y: a cationic or zwitterionic head group in component B;
(II) compounding of supermolecule antiscaling agent
Continuously adding 4-6.5 wt% of solubilizer, 2-3 wt% of complexing agent and 2-3 wt% of stripping agent, and stirring at normal temperature for 2-3h to obtain the compound supramolecular scale inhibitor.
The solubilizer is a halogen salt, and further comprises potassium chloride, sodium chloride, potassium bromide and/or sodium bromide.
The complexing agent comprises amino carboxylate, hydroxyl carboxylate, organic phosphonate, polyacrylic acid, phosphate, alcohol amine and/or sodium gluconate.
The stripping agent is a cationic surfactant containing large pi bonds, and further comprises alkyl phenyl dimethyl ammonium chloride with 8-18 carbon atoms and brominated alkyl pyridine with 8-18 carbon atoms.
Example 1
A synthesis method of macrocyclic compound supermolecule scale-dissolving material comprises the following steps:
preparation of supramolecular inclusion body
Adding a proper amount of beta-cyclodextrin, hexadecyl 3 methyl ammonium chloride, ethylene glycol and water into a three-neck flask, wherein the molar ratio of the beta-cyclodextrin: hexadecyl 3 methylammonium chloride ═ 1: 1.1, the mass ratio of reactants to glycol and water (mass of beta cyclodextrin + mass of hexadecyl 3 methyl ammonium chloride) to the mass of glycol: the water mass is 40:5: 45. Stirring and heating to 70 ℃, and reacting for 3h to obtain a mixture containing the supramolecular inclusion body.
(II) compounding of supermolecule antiscaling agent
Continuously adding potassium chloride, ethylene diamine tetraacetic acid tetrasodium salt and dodecyl dimethyl benzyl ammonium chloride into the mixture containing the supramolecular inclusion body, wherein the mass ratio of the mixture containing the supramolecular inclusion body is as follows: potassium chloride: ethylenediaminetetraacetic acid tetrasodium salt: dodecyl dimethyl benzyl ammonium chloride ═ 90: 5: 2.5: and 2.5, stirring for 2 hours at normal temperature to obtain the compound supermolecule scale dissolving solution.
Example 2
A synthesis method of macrocyclic compound supermolecule scale-dissolving material comprises the following steps:
preparation of supramolecular inclusion body
Adding appropriate amounts of 18-crown (ether) -6, hexadecyl dimethyl betaine, 1, 2-propylene glycol and water into a three-neck flask, wherein the molar ratio of reactants is 18-crown (ether) -6: hexadecyl dimethyl betaine ═ 1: 1.1, the mass ratio of reactants to 1,2 propylene glycol and water is (18-crown (ether) -6 mass + hexadecyl dimethyl betaine) to the mass of ethylene glycol: the water mass is 40:5: 45. Stirring and heating to 65 ℃, and reacting for 2h to obtain a mixture containing the supramolecular inclusion body.
(II) compounding of supermolecule antiscaling agent
Continuously adding sodium chloride, sodium gluconate and bromo-12 alkyl pyridine into the mixture containing the supramolecular inclusion body, wherein the mass ratio of the mixture containing the supramolecular inclusion body to the sodium chloride: sodium gluconate: bromo 12 alkyl pyridine ═ 90: 5: 2.5: and 2.5, stirring for 2 hours at normal temperature to obtain the compound supermolecule scale dissolving solution.
Example 3
Testing the scale prevention performance of the macrocyclic compound supramolecular scale inhibitor:
the performance of the scale inhibitor is evaluated by using the supramolecular scale solution in the embodiment 1 according to the petroleum industry standard SY/T5673, the addition amount of the scale inhibitor is 25mg/l, and the scale inhibitor rate reaches 90% at the temperature of 60 ℃, which is more than the technical requirement that the industrial scale inhibitor rate is more than 85%.
The supermolecule antiscaling agent is applied to the YJB-DT gathering and transportation pipeline of the JS oil field, the gathering and transportation pipeline contains barium and strontium scales, the pipeline needs to be cleaned every 6 months, the production is seriously influenced, the supermolecule antiscaling liquid is added according to the addition of 25mg/l, the gathering and transportation pipeline runs for 12 months safely and runs normally, and a better antiscaling effect is obtained.
Example 4
Testing the scale prevention performance of the macrocyclic compound supramolecular scale inhibitor:
200ml of 12% aqueous solution with the pH value of 9 was prepared by using the supramolecular scale inhibitor of example 2, 1g of barium sulfate scale was added and dissolved for 72 hours at 60 ℃, and the scale removal rate was 87%.
The JS oil field CH 3C 3-X well section is (2832.7-2842.9) m, the thickness is 10.2m, the average porosity is 18%, and the average permeability is 65 × 10-3μm2Belongs to a mesopore-mesopore reservoir, and the formation temperature is 99 ℃. Because of barium and strontium scales on a shaft and a perforation hole, the yield is obviously reduced. The well uses the supermolecule scale inhibitor compound formula of the embodiment 2 in 2019 and 3 months to prepare a scale dissolving solution of 30m3The supermolecule antiscaling agent 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 dissolution is increased to 4.4t/d from 2.5t/d before scale dissolution, and the oil increasing effect is obvious.
Claims (10)
1. A synthesis method of macrocyclic compound supermolecule scale-dissolving material is characterized by comprising the following steps:
preparation of supramolecular inclusion body
Adding a component A, a component B, a component C and water into a reaction container, wherein the molar ratio of the component A to the component B is 1: (1-1.3), the mass ratio of the (component A + the component B), the component C and the water is (38-42) to (4-6) to (40-48), stirring and heating to (60-70) DEG C, and reacting for (2-3) h to obtain a mixture containing a supramolecular inclusion body;
wherein the component A is a macrocyclic compound, and comprises beta cyclodextrin, gamma cyclodextrin, 18-crown-6 ether, calix [6] arene and calix [8] arene;
component B is selected from quaternary ammonium salt cationic surfactants and zwitterionic surfactants with 12-18 carbon atoms and a hydrophobic tail chain.
Component C is selected from low molecular weight alcohols, such as ethylene glycol, n-butanol and/or 1,2 propylene glycol;
(II) compounding of supermolecule antiscaling agent
Continuously adding 4-6.5 wt% of solubilizer, 2-3 wt% of complexing agent and 2-3 wt% of stripping agent, and stirring at normal temperature for 2-3h to obtain the compound supramolecular scale inhibitor.
2. The method of claim 1, wherein the solubilizing agent is a halogen salt, further comprising potassium chloride, sodium chloride, potassium bromide, and/or sodium bromide.
3. The synthesis method according to claim 1, wherein the complexing agent comprises aminocarboxylates, hydroxycarboxylic acids, organic phosphonates, polyacrylics, phosphates, alcohol amines and/or sodium gluconate.
4. The synthesis method according to claim 1, wherein the stripping agent is a cationic surfactant containing large pi bonds, and further comprises alkyl phenyl dimethyl ammonium chloride with 8-18 carbon atoms and alkyl bromide pyridine with 8-18 carbon atoms.
5. The synthesis method according to claim 1, wherein in the step (one), the molar ratio of the component A to the component B is 1: 1.1.
in the step (I), the mass ratio of the component A plus the component B to the component C to the water is 40:5: 45.
In the step (II), the mass ratio of the solubilizer to the complexing agent to the stripping agent is 2:1: 1.
6. Supramolecular antiscalants prepared by the synthesis method according to any one of claims 1 to 5.
7. Use of the supramolecular antiscalant according to claim 6 for descaling in oilfield pipelines.
8. Use according to claim 7, wherein the anti-scaling agent is added in the descaling of a gathering line in an amount of 25mg/l at a temperature of 60 degrees Celsius.
9. Use of the supramolecular antiscalant as claimed in claim 6 for descaling in oil field wellbores and perforations.
10. Use according to claim 9, characterized in that a 12% by weight solution of supramolecular antiscalant in water is formulated at 30m3Injecting from the oil casing annulus, closing the well and pumping out after 72 hours.
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| CN113913177A (en) * | 2021-12-13 | 2022-01-11 | 胜利油田新海兴达实业集团有限责任公司 | Composite acid for oil field oil-water well and preparation method thereof |
| CN116716091A (en) * | 2023-08-03 | 2023-09-08 | 东营市百扬石油科技有限责任公司 | Detergent composition and preparation method thereof |
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| CN113913177A (en) * | 2021-12-13 | 2022-01-11 | 胜利油田新海兴达实业集团有限责任公司 | Composite acid for oil field oil-water well and preparation method thereof |
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