CN112725804A - High-efficiency corrosion inhibitor for resisting carbon dioxide corrosion and preparation method thereof - Google Patents
High-efficiency corrosion inhibitor for resisting carbon dioxide corrosion and preparation method thereof Download PDFInfo
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- 238000005260 corrosion Methods 0.000 title claims abstract description 160
- 230000007797 corrosion Effects 0.000 title claims abstract description 160
- 239000003112 inhibitor Substances 0.000 title claims abstract description 80
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 34
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 122
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 73
- -1 imidazoline amide salt Chemical class 0.000 claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 66
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 49
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 45
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 230000005764 inhibitory process Effects 0.000 claims abstract description 34
- 239000005639 Lauric acid Substances 0.000 claims abstract description 31
- 239000005711 Benzoic acid Substances 0.000 claims abstract description 17
- 238000007112 amidation reaction Methods 0.000 claims abstract description 17
- 235000010233 benzoic acid Nutrition 0.000 claims abstract description 17
- 239000008096 xylene Substances 0.000 claims abstract description 17
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 230000018044 dehydration Effects 0.000 claims abstract description 6
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 6
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003129 oil well Substances 0.000 claims abstract description 6
- 230000006872 improvement Effects 0.000 claims abstract description 5
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 5
- 238000009833 condensation Methods 0.000 claims abstract description 3
- 230000005494 condensation Effects 0.000 claims abstract description 3
- 238000007363 ring formation reaction Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 112
- 238000010438 heat treatment Methods 0.000 claims description 70
- 238000003756 stirring Methods 0.000 claims description 70
- 238000000034 method Methods 0.000 claims description 62
- 239000007787 solid Substances 0.000 claims description 56
- 239000000203 mixture Substances 0.000 claims description 45
- 229920000805 Polyaspartic acid Polymers 0.000 claims description 43
- 108010064470 polyaspartate Proteins 0.000 claims description 43
- 238000001816 cooling Methods 0.000 claims description 28
- 238000003760 magnetic stirring Methods 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 28
- 239000008399 tap water Substances 0.000 claims description 28
- 235000020679 tap water Nutrition 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 238000005303 weighing Methods 0.000 claims description 22
- 230000000694 effects Effects 0.000 claims description 19
- 230000000844 anti-bacterial effect Effects 0.000 claims description 16
- 239000003899 bactericide agent Substances 0.000 claims description 16
- 239000003755 preservative agent Substances 0.000 claims description 16
- 230000002335 preservative effect Effects 0.000 claims description 16
- 229940123973 Oxygen scavenger Drugs 0.000 claims description 15
- ODHYIQOBTIWVRZ-UHFFFAOYSA-N n-propan-2-ylhydroxylamine Chemical compound CC(C)NO ODHYIQOBTIWVRZ-UHFFFAOYSA-N 0.000 claims description 15
- QQVGEJLUEOSDBB-KTKRTIGZSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(CO)(CO)CO QQVGEJLUEOSDBB-KTKRTIGZSA-N 0.000 claims description 14
- MGIYRDNGCNKGJU-UHFFFAOYSA-N isothiazolinone Chemical compound O=C1C=CSN1 MGIYRDNGCNKGJU-UHFFFAOYSA-N 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 238000005536 corrosion prevention Methods 0.000 claims description 4
- 238000013329 compounding Methods 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 239000013043 chemical agent Substances 0.000 abstract description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 24
- 238000011156 evaluation Methods 0.000 description 24
- 239000003921 oil Substances 0.000 description 16
- 230000033558 biomineral tissue development Effects 0.000 description 13
- 229910000975 Carbon steel Inorganic materials 0.000 description 12
- 239000010962 carbon steel Substances 0.000 description 12
- 238000011056 performance test Methods 0.000 description 12
- 229910052799 carbon Inorganic materials 0.000 description 11
- 230000008569 process Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000002455 scale inhibitor Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- UUIVKBHZENILKB-UHFFFAOYSA-N 2,2-dibromo-2-cyanoacetamide Chemical compound NC(=O)C(Br)(Br)C#N UUIVKBHZENILKB-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000008398 formation water Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009044 synergistic interaction Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/02—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in air or gases by adding vapour phase inhibitors
Abstract
The invention provides a high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion and a preparation method thereof, and relates to the field of chemical agents for tertiary oil recovery. The efficient corrosion inhibitor for resisting carbon dioxide corrosion and the preparation method thereof are based on the synthesis of a novel imidazoline amide salt, and on the basis, the efficient corrosion inhibitor is compounded with other environment-friendly water treatment agents to form an efficient corrosion inhibition system. The synthesis of the imidazoline amide salt corrosion inhibitor comprises two steps, wherein the first step is to uniformly mix lauric acid and diethylenetriamine according to a certain molar ratio, then add xylene as a water carrying agent, and obtain imidazoline triodes through high-temperature dehydration and cyclization reactions under the conditions of condensation and nitrogen introduction, and the second step is to add a proper amount of benzoic acid into the imidazoline triodes, and obtain imidazoline amide salt through high-temperature dehydration and amidation reactions. The corrosion inhibition rate of various high-temperature and high-pressure oil well pipelines can be greatly improved, so that the purposes of quality improvement and efficiency increase are achieved.
Description
Technical Field
The invention relates to the technical field of chemical agents for tertiary oil recovery, in particular to a high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion and a preparation method thereof.
Background
At present, CO is commonly used in various oil fields2Throughput technology for improving crude oil recovery ratio and CO2After being dissolved in formation water or injected with water, carbonic acid can be formed, which has strong corrosivity to oil gas production and transportation pipelines and equipment, and seriously threatens the safety of the petrochemical industry. To relieve CO2The most common method of corrosion problem is the addition of corrosion inhibitors. The imidazoline corrosion inhibitor is widely applied at present, but the selectivity of the corrosion inhibitor to the use environment is stronger, a single reagent cannot have good corrosion resistance at the same time, and the problems of incompatibility or poor cooperativity and the like exist among different reagents.
Under the background, a novel imidazoline amide salt corrosion inhibitor with more adsorption points, larger adsorption area and better water solubility is synthesized, a scale inhibitor polyaspartic acid, an oxygen scavenger N, N, N ', N' -tetra-substituted phenylenediamine and N-isopropyl hydroxylamine mixture and an environment-friendly bactericide dibromo nitrilo propionamide are compounded according to a certain proportion, a preservative sorbitol is added for prolonging the shelf life, the compounded corrosion inhibitor system can effectively reduce the content of bacteria and the content of oxygen in water and prevent scaling, the corrosion inhibition rate is greatly improved under the synergistic effect of the four components, the replacement cost of pipeline corrosion is saved, and the safety of field operation is also improved.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion and a preparation method thereof, and solves the problems that the imidazoline corrosion inhibitor has short effective period, is easy to be adsorbed and failed by rock strata in the stratum and has unsatisfactory corrosion prevention effect in the use process of carbon dioxide huff and puff.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation method of a high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion.
The method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.1-0.2%, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.3g to 0.6g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 1.5 to 2 hours to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 80-100mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.04g to 0.05g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 20 to 30min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of polyaspartic acid solution with the concentration of 0.1-0.2%, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 20-30min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 20-30min under magnetic stirring until the mixture is uniform to obtain a finished product.
Preferably, the preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: weighing 80-90g of lauric acid and 100-115g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 100-115g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 5-15g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 170-190 ℃, reacting for 2-4 hours at the temperature, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 20-30min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: 160g of products obtained in the steps are 150-160g, 170g of benzoic acid is added from the dropping funnel, the condensing device is connected, heating and stirring are started, meanwhile, nitrogen is introduced, heating and nitrogen introduction are stopped when the temperature reaches 150-170 ℃, the reaction is kept for 1-3 h at the temperature, and the viscous imidazoline amide salt is obtained after cooling.
Preferably, the starting point is to synthesize a novel imidazoline amide salt, and on the basis, the high-efficiency corrosion inhibition system is formed by compounding with other environment-friendly water treatment agents.
Preferably, the synthesis of the imidazoline amide salt corrosion inhibitor comprises two steps, wherein the first step is to uniformly mix lauric acid and diethylenetriamine according to a certain molar ratio, then add xylene as a water carrying agent, perform high-temperature dehydration and cyclization reaction under the conditions of condensation and nitrogen introduction to obtain triimidazoline, and the second step is to add a proper amount of benzoic acid into the obtained triimidazoline, and perform high-temperature dehydration and amidation reaction to obtain the imidazoline amide salt.
Preferably, the product is compounded to obtain a high-efficiency corrosion inhibitor system, the high-efficiency corrosion inhibitor system is applied to the field of corrosion prevention of carbon dioxide huff and puff wells, has an obvious effect of relieving corrosion phenomena of oil well pipelines, and can greatly improve the corrosion inhibition rate of various high-temperature and high-pressure oil well pipelines, so that the purposes of quality improvement and efficiency improvement are achieved.
Preferably, the molecular structural formula of the amide salt is:
(III) advantageous effects
The invention provides a high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion and a preparation method thereof. The method has the following beneficial effects:
1. the environment-friendly high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion disclosed by the invention has the advantages that a plurality of water treatment agents (scale inhibitor, deoxidant, bactericide and preservative) are introduced, the corrosion inhibition effect is greatly improved through the synergistic interaction effect, the problems that the conventional corrosion inhibitor is short in effective period, easy to adsorb and lose efficacy in a stratum and unsatisfactory in corrosion prevention effect and the like in the handling and using process can be solved, the corrosion inhibition rate can be greatly improved, and the corrosion inhibitor has the advantages of high temperature and high pressure (the temperature is 90 ℃, the mineralization is 30636mg/L, CO is 30636mg/L2Pressure 4MPa) is increased from 80 percent to more than 90 percent, and the dosage is reduced by 30 to 40 percent compared with the conventional corrosion inhibitor.
2. The environment-friendly high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion has good compatibility with different types of produced water, obviously improves the corrosion inhibition effect when used in huff and puff wells in different blocks of a large port oil field, greatly reduces the corrosion speed of an oil well pipe column, saves the maintenance and replacement cost, and improves the safety of field operation.
3. All the medicaments in the invention are environment-friendly nontoxic products, meet the requirement of environmental protection, do not cause harm to human bodies in the using process, and simultaneously do not cause water body pollution and stratum damage, thus being a green and environment-friendly medicament.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
the preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion comprises the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.1 percent, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.3g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 1.5h to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 80mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.04g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 20min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of 0.1% polyaspartic acid solution, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 20min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 20min under magnetic stirring until the mixture is uniform to obtain a finished product.
(2) The preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: weighing 85g of lauric acid and 110g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 110g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 5g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 170 ℃, keeping the temperature for reaction for 2 hours, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 20min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: and adding 160g of benzoic acid from a dropping funnel, connecting a condensing device, starting heating and stirring, introducing nitrogen gas, stopping heating and introducing nitrogen gas when the temperature reaches 150 ℃, keeping the temperature for reacting for 1.5h, and cooling to obtain the viscous imidazoline amide salt, wherein the mass of the product obtained in the step is about 150 g.
Evaluation of Performance test
The produced water (degree of mineralization 30363mg/L) of a certain block of the Hongkong oil field is selected as an evaluation medium, and the stratum temperature and the stratum pressure (temperature 90 ℃, CO) of the block are2Partial pressure 4MPa, total pressure 10MPa) as experimental conditions. The environment-friendly high-efficiency corrosion inhibitor is prepared into a solution with the concentration of 100mg/L, the dynamic corrosion inhibition rate of the environment-friendly high-efficiency corrosion inhibitor in different time periods under the conditions of high temperature and high pressure is evaluated by a high-temperature high-pressure dynamic corrosion instrument (the size of an N80 carbon steel hanging piece is 60mm multiplied by 10mm multiplied by 3mm), and the effect of improving the corrosion inhibition rate is obvious by comparing with the conventional corrosion inhibitor. The results are shown in the following table:
example two:
the preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion comprises the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.15%, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.45g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 2 hours to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 90mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.045g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 20min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of 0.15% polyaspartic acid solution, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 20min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 25min under magnetic stirring until the mixture is uniform to obtain a finished product.
(2) The preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: weighing 85g of lauric acid and 110g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 110g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 5g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 170 ℃, keeping the temperature for reaction for 2 hours, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 20min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: and adding 160g of benzoic acid from a dropping funnel, connecting a condensing device, starting heating and stirring, introducing nitrogen gas, stopping heating and introducing nitrogen gas when the temperature reaches 150 ℃, keeping the temperature for reacting for 1.5h, and cooling to obtain the viscous imidazoline amide salt, wherein the mass of the product obtained in the step is about 150 g.
(3) Evaluation of Performance test
The produced water (degree of mineralization 30363mg/L) of a certain block of the Hongkong oil field is selected as an evaluation medium, and the stratum temperature and the stratum pressure (temperature 90 ℃, CO) of the block are2Partial pressure 4MPa, total pressure 10MPa) as experimental conditions. The environment-friendly high-efficiency corrosion inhibitor is prepared into a solution with the concentration of 100mg/L, the dynamic corrosion inhibition rate of the environment-friendly high-efficiency corrosion inhibitor in different time periods under the conditions of high temperature and high pressure is evaluated by a high-temperature high-pressure dynamic corrosion instrument (the size of an N80 carbon steel hanging piece is 60mm multiplied by 10mm multiplied by 3mm), and the effect of improving the corrosion inhibition rate is obvious by comparing with the conventional corrosion inhibitor. The results are shown in the following table:
example three:
the preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion comprises the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.2 percent, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.6g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 2 hours to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 100mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.05g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 30min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of 0.2% polyaspartic acid solution, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 30min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 30min under magnetic stirring until the mixture is uniform to obtain a finished product.
(2) The preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: weighing 85g of lauric acid and 110g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 110g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 5g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 170 ℃, keeping the temperature for reaction for 2 hours, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 20min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: and adding 160g of benzoic acid from a dropping funnel, connecting a condensing device, starting heating and stirring, introducing nitrogen gas, stopping heating and introducing nitrogen gas when the temperature reaches 150 ℃, keeping the temperature for reacting for 1.5h, and cooling to obtain the viscous imidazoline amide salt, wherein the mass of the product obtained in the step is about 150 g.
(3) Evaluation of Performance test
The produced water (degree of mineralization 30363mg/L) of a certain block of the Hongkong oil field is selected as an evaluation medium, and the stratum temperature and the stratum pressure (temperature 90 ℃, CO) of the block are2Partial pressure 4MPa, total pressure 10MPa) as experimental conditions. The high-efficiency corrosion inhibitor is prepared into a solution with the concentration of 100mg/L, the dynamic corrosion inhibition rate of the high-efficiency corrosion inhibitor in different time periods under the conditions of high temperature and high pressure is evaluated by a high-temperature high-pressure dynamic corrosion meter (the size of an N80 carbon steel hanging piece is 60mm multiplied by 10mm multiplied by 3mm), and the effect of improving the corrosion inhibition rate is obvious by comparing with the conventional corrosion inhibitor. The results are shown in the following table:
example four:
the preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion comprises the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.1 percent, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.3g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 1.5h to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 80mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.04g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 20min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of 0.1% polyaspartic acid solution, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 20min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 20min under magnetic stirring until the mixture is uniform to obtain a finished product.
(2) The preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: measuring 90g of lauric acid and 100g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 100g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 10g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 180 ℃, keeping the temperature for reaction for 3 hours, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 25min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: and adding 165g of benzoic acid from a dropping funnel, connecting a condensing device, starting heating and stirring, introducing nitrogen gas, stopping heating and introducing nitrogen gas when the temperature reaches 160 ℃, keeping the temperature for reaction for 2 hours, and cooling to obtain the viscous imidazoline amide salt, wherein the mass of the product obtained in the step is about 155 g.
Evaluation of Performance test
The produced water (degree of mineralization 30363mg/L) of a certain block of the Hongkong oil field is selected as an evaluation medium, and the stratum temperature and the stratum pressure (temperature 90 ℃, CO) of the block are2Partial pressure 4MPa, total pressure 10MPa) as experimental conditions. The high-efficiency corrosion inhibitor is prepared into a solution with the concentration of 100mg/L, the dynamic corrosion inhibition rate of the high-efficiency corrosion inhibitor in different time periods under the conditions of high temperature and high pressure is evaluated by a high-temperature high-pressure dynamic corrosion meter (the size of an N80 carbon steel hanging piece is 60mm multiplied by 10mm multiplied by 3mm), and the effect of improving the corrosion inhibition rate is obvious by comparing with the conventional corrosion inhibitor. The results are shown in the following table:
example five:
the preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion comprises the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.15%, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.45g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 2 hours to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 90mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.045g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 20min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of 0.15% polyaspartic acid solution, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 20min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 25min under magnetic stirring until the mixture is uniform to obtain a finished product.
(2) The preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: measuring 90g of lauric acid and 100g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 100g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 10g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 180 ℃, keeping the temperature for reaction for 3 hours, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 25min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: and adding 165g of benzoic acid from a dropping funnel, connecting a condensing device, starting heating and stirring, introducing nitrogen gas, stopping heating and introducing nitrogen gas when the temperature reaches 160 ℃, keeping the temperature for reaction for 2 hours, and cooling to obtain the viscous imidazoline amide salt, wherein the mass of the product obtained in the step is about 155 g.
(3) Evaluation of Performance test
The produced water (degree of mineralization 30363mg/L) of a certain block of the Hongkong oil field is selected as an evaluation medium, and the stratum temperature and the stratum pressure (temperature 90 ℃, CO) of the block are2Partial pressure 4MPa, total pressure 10MPa) as experimental conditions. The high-efficiency corrosion inhibitor is prepared into a solution with the concentration of 100mg/L, the dynamic corrosion inhibition rate of the high-efficiency corrosion inhibitor in different time periods under the conditions of high temperature and high pressure (the size of an N80 carbon steel hanging piece is 60mm multiplied by 10mm multiplied by 3mm) is evaluated by a high-temperature high-pressure dynamic corrosion meterCompared with the conventional corrosion inhibitor, the corrosion inhibition rate is obviously improved. The results are shown in the following table:
example six:
the preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion comprises the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.2 percent, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.6g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 2 hours to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 100mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.05g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 30min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of 0.2% polyaspartic acid solution, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 30min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 30min under magnetic stirring until the mixture is uniform to obtain a finished product.
(2) The preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: measuring 90g of lauric acid and 100g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 100g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 10g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 180 ℃, keeping the temperature for reaction for 3 hours, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 25min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: and adding 165g of benzoic acid from a dropping funnel, connecting a condensing device, starting heating and stirring, introducing nitrogen gas, stopping heating and introducing nitrogen gas when the temperature reaches 160 ℃, keeping the temperature for reaction for 2 hours, and cooling to obtain the viscous imidazoline amide salt, wherein the mass of the product obtained in the step is about 155 g.
(3) Evaluation of Performance test
The produced water (degree of mineralization 30363mg/L) of a certain block of the Hongkong oil field is selected as an evaluation medium, and the stratum temperature and the stratum pressure (temperature 90 ℃, CO) of the block are2Partial pressure 4MPa, total pressure 10MPa) as experimental conditions. The high-efficiency corrosion inhibitor is prepared into a solution with the concentration of 100mg/L, the dynamic corrosion inhibition rate of the high-efficiency corrosion inhibitor in different time periods under the conditions of high temperature and high pressure is evaluated by a high-temperature high-pressure dynamic corrosion meter (the size of an N80 carbon steel hanging piece is 60mm multiplied by 10mm multiplied by 3mm), and the effect of improving the corrosion inhibition rate is obvious by comparing with the conventional corrosion inhibitor. The results are shown in the following table:
example seven:
the preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion comprises the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.1 percent, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.3g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 1.5h to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 80mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.04g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 20min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of 0.1% polyaspartic acid solution, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 30min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 20min under magnetic stirring until the mixture is uniform to obtain a finished product.
(2) The preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: measuring 95g of lauric acid and 100g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 100g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 5g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 190 ℃, reacting for 3.5 hours at the temperature, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 25min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: and adding 170g of benzoic acid into the dropping funnel, connecting a condensing device, starting heating and stirring, introducing nitrogen gas, stopping heating and introducing nitrogen gas when the temperature reaches 170 ℃, keeping the temperature for reacting for 2 hours, and cooling to obtain the viscous imidazoline amide salt, wherein the mass of the product obtained in the step is about 160 g.
(3) Evaluation of Performance test
Selecting a certain oil field in a large portProduced water (degree of mineralization 30363mg/L) of the block was used as the evaluation medium, and formation temperature and pressure (temperature 90 ℃, CO) of the block2Partial pressure 4MPa, total pressure 10MPa) as experimental conditions. The high-efficiency corrosion inhibitor is prepared into a solution with the concentration of 100mg/L, the dynamic corrosion inhibition rate of the high-efficiency corrosion inhibitor in different time periods under the conditions of high temperature and high pressure is evaluated by a high-temperature high-pressure dynamic corrosion meter (the size of an N80 carbon steel hanging piece is 60mm multiplied by 10mm multiplied by 3mm), and the effect of improving the corrosion inhibition rate is obvious by comparing with the conventional corrosion inhibitor. The results are shown in the following table:
example eight:
the preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion comprises the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.15%, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.45g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 1.5h to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 90mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.045g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 30min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of 0.15% polyaspartic acid solution, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 20min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 30min under magnetic stirring until the mixture is uniform to obtain a finished product.
(2) The preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: measuring 95g of lauric acid and 100g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 100g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 5g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 190 ℃, reacting for 3.5 hours at the temperature, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 25min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: and adding 170g of benzoic acid into the dropping funnel, connecting a condensing device, starting heating and stirring, introducing nitrogen gas, stopping heating and introducing nitrogen gas when the temperature reaches 170 ℃, keeping the temperature for reacting for 2 hours, and cooling to obtain the viscous imidazoline amide salt, wherein the mass of the product obtained in the step is about 160 g.
(3) Evaluation of Performance test
The produced water (degree of mineralization 30363mg/L) of a certain block of the Hongkong oil field is selected as an evaluation medium, and the stratum temperature and the stratum pressure (temperature 90 ℃, CO) of the block are2Partial pressure 4MPa, total pressure 10MPa) as experimental conditions. The high-efficiency corrosion inhibitor is prepared into a solution with the concentration of 100mg/L, the dynamic corrosion inhibition rate of the high-efficiency corrosion inhibitor in different time periods under the conditions of high temperature and high pressure is evaluated by a high-temperature high-pressure dynamic corrosion meter (the size of an N80 carbon steel hanging piece is 60mm multiplied by 10mm multiplied by 3mm), and the effect of improving the corrosion inhibition rate is obvious by comparing with the conventional corrosion inhibitor. The results are shown in the following table:
example nine:
the preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion comprises the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.2 percent, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.6g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 2 hours to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 100mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.05g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 30min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of 0.2% polyaspartic acid solution, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 30min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 30min under magnetic stirring until the mixture is uniform to obtain a finished product.
(2) The preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: measuring 95g of lauric acid and 100g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 100g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 5g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 190 ℃, reacting for 3.5 hours at the temperature, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 25min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: and adding 170g of benzoic acid into the dropping funnel, connecting a condensing device, starting heating and stirring, introducing nitrogen gas, stopping heating and introducing nitrogen gas when the temperature reaches 170 ℃, keeping the temperature for reacting for 2 hours, and cooling to obtain the viscous imidazoline amide salt, wherein the mass of the product obtained in the step is about 160 g.
(3) Evaluation of Performance test
The produced water (degree of mineralization 30363mg/L) of a certain block of the Hongkong oil field is selected as an evaluation medium, and the stratum temperature and the stratum pressure (temperature 90 ℃, CO) of the block are2Partial pressure 4MPa, total pressure 10MPa) as experimental conditions. The high-efficiency corrosion inhibitor is prepared into a solution with the concentration of 100mg/L, the dynamic corrosion inhibition rate of the high-efficiency corrosion inhibitor in different time periods under the conditions of high temperature and high pressure is evaluated by a high-temperature high-pressure dynamic corrosion meter (the size of an N80 carbon steel hanging piece is 60mm multiplied by 10mm multiplied by 3mm), and the effect of improving the corrosion inhibition rate is obvious by comparing with the conventional corrosion inhibitor. The results are shown in the following table:
example ten:
the preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion comprises the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.1 percent, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.3g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 1.5h to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 80mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.04g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 20min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of 0.1% polyaspartic acid solution, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 20min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 20min under magnetic stirring until the mixture is uniform to obtain a finished product.
(2) The preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: weighing 80g of lauric acid and 110g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 110g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 10g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 190 ℃, reacting for 4 hours at the temperature, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 25min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: and adding 170g of benzoic acid into the dropping funnel, connecting a condensing device, starting heating and stirring, introducing nitrogen gas, stopping heating and introducing nitrogen gas when the temperature reaches 170 ℃, keeping the temperature for reacting for 3 hours, and cooling to obtain the viscous imidazoline amide salt, wherein the mass of the product obtained in the step is about 160 g.
(3) Evaluation of Performance test
The produced water (the degree of mineralization is 30363mg/L) of a certain block of the Hongkong oil field is selected as an evaluation medium, and the formation temperature and the formation pressure (the temperature) of the block areTemperature of 90 ℃ and CO2Partial pressure 4MPa, total pressure 10MPa) as experimental conditions. The high-efficiency corrosion inhibitor is prepared into a solution with the concentration of 100mg/L, the dynamic corrosion inhibition rate of the high-efficiency corrosion inhibitor in different time periods under the conditions of high temperature and high pressure is evaluated by a high-temperature high-pressure dynamic corrosion meter (the size of an N80 carbon steel hanging piece is 60mm multiplied by 10mm multiplied by 3mm), and the effect of improving the corrosion inhibition rate is obvious by comparing with the conventional corrosion inhibitor. The results are shown in the following table:
example eleven:
the preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion comprises the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.15%, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.45g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 1.5h to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 90mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.045g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 30min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of 0.15% polyaspartic acid solution, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 20min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 25min under magnetic stirring until the mixture is uniform to obtain a finished product.
(2) The preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: weighing 80g of lauric acid and 110g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 110g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 10g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 190 ℃, reacting for 4 hours at the temperature, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 25min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: and adding 170g of benzoic acid into the dropping funnel, connecting a condensing device, starting heating and stirring, introducing nitrogen gas, stopping heating and introducing nitrogen gas when the temperature reaches 170 ℃, keeping the temperature for reacting for 3 hours, and cooling to obtain the viscous imidazoline amide salt, wherein the mass of the product obtained in the step is about 160 g.
(3) Evaluation of Performance test
The produced water (degree of mineralization 30363mg/L) of a certain block of the Hongkong oil field is selected as an evaluation medium, and the stratum temperature and the stratum pressure (temperature 90 ℃, CO) of the block are2Partial pressure 4MPa, total pressure 10MPa) as experimental conditions. The high-efficiency corrosion inhibitor is prepared into a solution with the concentration of 100mg/L, the dynamic corrosion inhibition rate of the high-efficiency corrosion inhibitor in different time periods under the conditions of high temperature and high pressure is evaluated by a high-temperature high-pressure dynamic corrosion meter (the size of an N80 carbon steel hanging piece is 60mm multiplied by 10mm multiplied by 3mm), and the effect of improving the corrosion inhibition rate is obvious by comparing with the conventional corrosion inhibitor. The results are shown in the following table:
example twelve:
the preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion comprises the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.2 percent, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.45g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 2 hours to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 100mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.05g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 30min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of 0.2% polyaspartic acid solution, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 30min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 30min under magnetic stirring until the mixture is uniform to obtain a finished product.
(2) The preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: weighing 80g of lauric acid and 110g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 110g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 10g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 190 ℃, reacting for 4 hours at the temperature, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 25min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: and adding 170g of benzoic acid into the dropping funnel, connecting a condensing device, starting heating and stirring, introducing nitrogen gas, stopping heating and introducing nitrogen gas when the temperature reaches 170 ℃, keeping the temperature for reacting for 3 hours, and cooling to obtain the viscous imidazoline amide salt, wherein the mass of the product obtained in the step is about 160 g.
(3) Evaluation of Performance test
The produced water (degree of mineralization 30363mg/L) of a certain block of the Hongkong oil field is selected as an evaluation medium, and the stratum temperature and the stratum pressure (temperature 90 ℃, CO) of the block are2Partial pressure 4MPa, total pressure 10MPa) as experimental conditions. The high-efficiency corrosion inhibitor is prepared into a solution with the concentration of 100mg/L, the dynamic corrosion inhibition rate of the high-efficiency corrosion inhibitor in different time periods under the conditions of high temperature and high pressure is evaluated by a high-temperature high-pressure dynamic corrosion meter (the size of an N80 carbon steel hanging piece is 60mm multiplied by 10mm multiplied by 3mm), and the effect of improving the corrosion inhibition rate is obvious by comparing with the conventional corrosion inhibitor. The results are shown in the following table:
although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A preparation method of a high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion is characterized by comprising the following steps:
the method comprises the following steps: preparing solid polyaspartic acid into a solution with the mass concentration of 0.1-0.2%, and the specific method comprises the following steps: 300mL of tap water is filled in a 500mL beaker, a stirring device is started to enable the water surface to form a vortex, 0.3g to 0.6g of solid polyaspartic acid powder is uniformly added into the vortex at the rotating speed of 400r/min, and the stirring is continued for 1.5 to 2 hours to form uniform liquid.
Step two: preparing a solid deoxidant N, N, N ', N' -tetra-substituted phenylenediamine into a solution with the mass concentration of 80-100mg/L, and the specific method comprises the following steps: 500mL of tap water is filled in a 1000mL beaker, the beaker is placed on a magnetic stirrer, 0.04g to 0.05g of solid deoxidant is uniformly added into the beaker at the rotating speed of 400r/min, and the beaker is stirred for 20 to 30min to be completely dissolved to form uniform liquid. And taking out 100g of the uniform liquid, adding 70g of liquid deoxidant N-isopropyl hydroxylamine, and uniformly mixing to obtain deoxidant mixture.
Step three: 100g of polyaspartic acid solution with the concentration of 0.1-0.2%, 60g of oxygen scavenger mixture, 50g of liquid bactericide isothiazolinone and 30g of liquid preservative pentaerythritol monooleate are sequentially added into a 500mL beaker and stirred for 20-30min to be uniform under magnetic stirring.
Step four: and (3) transferring all the liquid in the third step into a 1000mL beaker, adding 300g of liquid imidazoline amide salt into the beaker, and stirring for 20-30min under magnetic stirring until the mixture is uniform to obtain a finished product.
2. The preparation method of the high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion according to claim 1, which is characterized by comprising the following steps: the preparation method of the imidazoline amide salt comprises the following steps:
the method comprises the following steps: weighing 80-90g of lauric acid and 100-115g of diethylenetriamine by the total mass of 200g, adding the lauric acid and 100-115g of diethylenetriamine into a four-neck flask provided with a mechanical stirrer, a condenser pipe, a dropping funnel, a nitrogen introducing device, a pressure reducing device and a water separator, uniformly mixing, and connecting a condensing device; weighing 5-15g of dimethylbenzene, adding the dimethylbenzene into the four-neck flask, starting heating and stirring, introducing nitrogen, stopping heating and introducing nitrogen when the temperature reaches 170-190 ℃, reacting for 2-4 hours at the temperature, and stopping reaction after no water is generated, so as to obtain a triomidazoline product.
Step two: and opening a pressure reducing device, distilling under reduced pressure for 20-30min under heating, distilling out excessive xylene and diethylenetriamine, and carrying out the next amidation reaction after proper cooling.
Step three: 160g of products obtained in the steps are 150-160g, 170g of benzoic acid is added from the dropping funnel, the condensing device is connected, heating and stirring are started, meanwhile, nitrogen is introduced, heating and nitrogen introduction are stopped when the temperature reaches 150-170 ℃, the reaction is kept for 1-3 h at the temperature, and the viscous imidazoline amide salt is obtained after cooling.
3. The high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion and the preparation method thereof according to claim 1 are characterized in that: the method takes the synthesis of a novel imidazoline amide salt as a starting point, and forms a high-efficiency corrosion inhibition system by compounding with other environment-friendly water treatment agents on the basis.
4. The high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion and the preparation method thereof according to claim 1 are characterized in that: the synthesis of the imidazoline amide salt corrosion inhibitor comprises two steps, wherein the first step is to uniformly mix lauric acid and diethylenetriamine according to a certain molar ratio, then add xylene as a water carrying agent, and obtain imidazoline triodes through high-temperature dehydration and cyclization reactions under the conditions of condensation and nitrogen introduction, and the second step is to add a proper amount of benzoic acid into the imidazoline triodes, and obtain imidazoline amide salt through high-temperature dehydration and amidation reactions.
5. The high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion and the preparation method thereof according to claim 1 are characterized in that: the high-efficiency corrosion inhibitor system is obtained after compounding the product, is applied to the field of corrosion prevention of carbon dioxide huff-puff wells, has an obvious effect of relieving corrosion phenomena of oil well pipelines, and can greatly improve the corrosion inhibition rate of various high-temperature and high-pressure oil well pipelines, so that the purposes of quality improvement and efficiency improvement are achieved.
6. The high-efficiency corrosion inhibitor for resisting carbon dioxide corrosion and the preparation method thereof according to claim 1 are characterized in that: the molecular structural formula of the amide salt is as follows:
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