CN114716990B - Oilfield high Wen Fanggou corrosion inhibitor and preparation method thereof - Google Patents

Oilfield high Wen Fanggou corrosion inhibitor and preparation method thereof Download PDF

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CN114716990B
CN114716990B CN202210102540.5A CN202210102540A CN114716990B CN 114716990 B CN114716990 B CN 114716990B CN 202210102540 A CN202210102540 A CN 202210102540A CN 114716990 B CN114716990 B CN 114716990B
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alkenyl
temperature
sulfonic acid
fanggou
mass
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CN114716990A (en
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陆原
张勇
易飞
张晓灵
陈胜利
刘言霞
张妙玮
张国欣
王超明
王勇
刘志光
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CNOOC Energy Technology and Services Ltd
CNOOC Tianjin Oilfield Chemical Co Ltd
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CNOOC Tianjin Oilfield Chemical Co Ltd
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Abstract

The invention discloses an oilfield high Wen Fanggou corrosion inhibitor. Compared with various currently used high Wen Fanggou corrosion inhibitors, the invention has higher efficient scale prevention and corrosion inhibition effects and better stability and high temperature resistance aiming at corrosion and scaling of offshore oilfield high-temperature production water and water injection.

Description

Oilfield high Wen Fanggou corrosion inhibitor and preparation method thereof
Technical Field
The invention belongs to the technical field of chemical scale and corrosion inhibition, relates to a scale and corrosion inhibitor, and in particular relates to an oilfield high Wen Fanggou corrosion inhibitor and a preparation method thereof.
Background
At present, some offshore oil fields begin to adopt underground dosing or water injection or thermal recovery operation after heating production water, although resources can be fully utilized and emission is reduced, scaling and corrosion problems are more serious, and currently common antiscaling agents such as sodium polyacrylate, sodium polyepoxysuccinate, multipolymer and the like have obviously reduced application effect after the temperature exceeds 100 ℃, and have no inhibition effect on corrosion. The corrosion inhibitor with good corrosion inhibition effect on high-temperature production water is a cationic nitrogen-containing compound and has obvious antagonism effect with the scale inhibitor, so that a novel scale and corrosion inhibitor needs to be developed to solve the problems of scaling and corrosion in the operation process. The invention improves the effect of high Wen Fanggou by copolymerization of a plurality of carboxylic acids, and simultaneously utilizes the condensation of amide groups in molecular chains, aldehyde and heterocyclic compounds to form nonionic corrosion inhibition functional groups resistant to high temperature corrosion, and then utilizes synergistic effect by compounding to obtain the oilfield high Wen Fanggou corrosion inhibitor with high temperature scaling resistance and corrosion resistance.
Disclosure of Invention
The invention aims to develop an oilfield high Wen Fanggou corrosion inhibitor, which can effectively relieve the scaling and corrosion of oilfield high temperature and the scaling and corrosion of a downhole tubular column. The anti-scaling agent has the characteristics of small dosage, good anti-scaling effect, high anti-scaling rate, high temperature resistance, stability, wide application range and the like.
The invention is realized by the following technical scheme:
an oilfield high Wen Fanggou corrosion inhibitor is prepared by the following steps:
firstly, adding equimolar alkenyl amide, alkenyl sulfonic acid, maleic anhydride and itaconic acid and distilled water which is 5 times of the total mass of the alkenyl amide, the alkenyl sulfonic acid, the maleic anhydride and the itaconic acid into a reaction container, starting stirring and continuously introducing nitrogen;
step two, respectively loading Acrylic Acid (AA) with the mass of 6-10 times of that of the alkenyl amide and hydrogen peroxide with the mass of 25-40% of that of the alkenyl amide in the reaction container into two high-level drip tanks;
step three, after introducing nitrogen into the reaction vessel for more than 15 minutes, adding sodium hypophosphite accounting for 25-40% of the mass of the alkenyl amide into the reaction vessel;
step four, heating is started, and after the temperature reaches more than 50 ℃, acrylic acid and hydrogen peroxide prepared in the step two are added dropwise at the same time, and the temperature is controlled to be not more than 90 ℃;
stopping introducing nitrogen after the dripping is finished, controlling the temperature to be 75-90 ℃ and reacting for 2-4 hours;
sequentially adding methyl nitrogenous heterocyclic compound with the mole ratio of alkenyl amide of 0.8:0.95, wherein the mass of anhydride with the mass of alkenyl amide of 10-20 percent, continuously controlling the temperature to be not more than 90 ℃, and dropwise adding formalin with the mole ratio of alkenyl amide of 1:1.05;
step seven, after the dripping is finished, reacting for 4 to 8 hours at the temperature of 80 to 95 ℃ to prepare an intermediate A;
step eight, reducing to normal temperature, adding polyamino polyether methylene Phosphonic Acid (PAPEMP) accounting for 20-30% of the total mass of the intermediate A, polyol Phosphonic Acid (PAPE) accounting for 20-30% of the total mass of the intermediate A, dodecyl dimethyl benzyl ammonium chloride accounting for 5-10% of the total mass of the intermediate A, and triethanolamine alkyl acid accounting for 0.1-0.5% of the total mass of the intermediate A, and stirring uniformly to obtain the high Wen Fanggou corrosion inhibitor.
In the above technical scheme, the alkenyl amide is acrylamide or methacrylamide.
In the above technical scheme, the alkenyl sulfonic acid is vinyl sulfonic acid, allyl sulfonic acid, propenyl sulfonic acid or butenyl sulfonic acid.
In the above technical scheme, the methyl nitrogen-containing heterocyclic compound is picoline, methylquinoline or methylimidazole.
In the technical scheme, the anhydride is formic anhydride, acetic anhydride or propionic anhydride.
In the above technical scheme, the alkyl acid triethanolamine is one or a mixture of two of benzoic acid triethanolamine, oleic acid triethanolamine and lauric acid triethanolamine.
The preparation method of the oilfield high Wen Fanggou corrosion inhibitor provided by the invention comprises the following steps:
firstly, adding equimolar alkenyl amide, alkenyl sulfonic acid, maleic anhydride and itaconic acid and distilled water which is 5 times of the total mass of the alkenyl amide, the alkenyl sulfonic acid, the maleic anhydride and the itaconic acid into a reaction container, starting stirring and continuously introducing nitrogen;
step two, respectively loading Acrylic Acid (AA) with the mass of 6-10 times of that of the alkenyl amide and hydrogen peroxide with the mass of 25-40% of that of the alkenyl amide in the reaction container into two high-level drip tanks;
step three, after introducing nitrogen into the reaction vessel for more than 15 minutes, adding sodium hypophosphite accounting for 25-40% of the mass of the alkenyl amide into the reaction vessel;
step four, heating is started, and after the temperature reaches more than 50 ℃, acrylic acid and hydrogen peroxide prepared in the step two are added dropwise at the same time, and the temperature is controlled to be not more than 90 ℃;
stopping introducing nitrogen after the dripping is finished, controlling the temperature to be 75-90 ℃ and reacting for 2-4 hours;
sequentially adding methyl nitrogenous heterocyclic compound with the mole ratio of alkenyl amide of 0.80:0.95, adding anhydride with the mass of 10-20% of that of alkenyl amide, continuously controlling the temperature to be not more than 90 ℃, and dropwise adding formalin with the mole ratio of alkenyl amide of 1:1.05;
step seven, after the dripping is finished, reacting for 4 to 8 hours at the temperature of 80 to 95 ℃ to prepare an intermediate A;
step eight, reducing to normal temperature, adding polyamino polyether methylene Phosphonic Acid (PAPEMP) accounting for 20-30% of the total mass of the intermediate A, adding polyol phosphonate (PAPE) accounting for 20-30% of the total mass of the intermediate A, adding dodecyl dimethyl benzyl ammonium chloride accounting for 5-10% of the total mass of the intermediate A, adding triethanolamine alkyl acid accounting for 0.1-0.5% of the total mass of the intermediate A, and stirring uniformly to obtain the high Wen Fanggou corrosion inhibitor.
The alkenyl amide is acrylamide or methacrylamide; the alkenyl sulfonic acid is vinyl sulfonic acid, allyl sulfonic acid, propenyl sulfonic acid or butenyl sulfonic acid; the methyl nitrogen-containing heterocyclic compound is picoline, methylquinoline or methylimidazole; the anhydride is formic anhydride, acetic anhydride or propionic anhydride; the alkyl acid triethanolamine is one or two of benzoic acid triethanolamine, oleic acid triethanolamine and lauric acid triethanolamine.
The invention has the advantages and beneficial effects that:
compared with various currently used high Wen Fanggou corrosion inhibitors, the invention has higher efficient scale prevention and corrosion inhibition effects and better stability and high temperature resistance aiming at corrosion and scaling of offshore oilfield high-temperature production water and water injection.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
Example 1:
(1) 71.08g of acrylamide (1 mol), 108.12g of vinylsulfonic acid (1 mol), 98.06g of maleic anhydride (1 mol) and 130.08g of itaconic acid, and 2036.7g of distilled water were charged into a reaction vessel, stirring was started and nitrogen gas was continuously introduced;
(2) 426.48g of Acrylic Acid (AA) (6 times) and 17.77g of hydrogen peroxide (25 percent) are respectively contained in two high-level drip tanks;
(3) after nitrogen is introduced into the reaction vessel for more than 15 minutes, 17.77g of sodium hypophosphite (25%) is added into the reaction vessel;
(4) starting heating, and dripping the acrylic acid and the hydrogen peroxide prepared in the second step after the temperature reaches more than 50 ℃, wherein the temperature is controlled to be not more than 90 ℃;
(5) stopping introducing nitrogen after the dripping is finished, controlling the temperature to be 75 ℃ and reacting for 4 hours;
(6) 136.03g of methylquinoline (0.95 mol) and 7.11g of formic anhydride (10%) are added in sequence, the temperature is kept at 90 ℃ and 85.22g of formalin (1.05 mol) are added dropwise;
(7) after the dripping is finished, reacting for 8 hours at 95 ℃ to prepare an intermediate A1;
(8) lowering the temperature to normal temperature, adding 626.88g of polyamino polyether methylene Phosphonic Acid (PAPEMP) (20%), 940.33g of polyol phosphonate (PAPE) (30%), 313.44g of dodecyl dimethyl benzyl ammonium chloride (10%), 3.13g of triethanolamine benzoate (0.1%), and stirring uniformly to obtain the high Wen Fanggou corrosion inhibitor B1.
Example 2:
(1) 71.08g of acrylamide (1 mol), 122.10g of allylsulfonic acid (1 mol), 98.06g of maleic anhydride (1 mol) and 130.08g of itaconic acid, and 2106.6g of distilled water were charged into a reaction vessel, stirring was started and nitrogen gas was continuously introduced;
(2) 710.80g of Acrylic Acid (AA) (10 times) and 28.43g of hydrogen peroxide (40 percent) are respectively contained in two high-level drip tanks;
(3) after the nitrogen is introduced into the reaction vessel for more than 15 minutes, 28.43g of sodium hypophosphite (40%) is added into the reaction vessel;
(4) starting heating, and dripping the acrylic acid and the hydrogen peroxide prepared in the second step after the temperature reaches more than 50 ℃, wherein the temperature is controlled to be not more than 90 ℃;
(5) stopping introducing nitrogen after the dripping is finished, controlling the temperature to be 75 ℃ and reacting for 4 hours;
(6) 65.68g of methylimidazole (0.80 mol) and 14.22g of propionic anhydride (20%) were added in sequence, and dropwise adding 81.16g of formalin (1.00 mol) at a temperature not exceeding 90℃was continued to be controlled;
(7) after the dripping is finished, reacting for 6 hours at 80 ℃ to prepare an intermediate A2;
(8) lowering the temperature to normal temperature, adding 1036.98g of polyamino polyether methylene Phosphonic Acid (PAPEMP) (30%), 691.32g of polyol phosphonate (PAPE) (20%), 172.83g of dodecyl dimethyl benzyl ammonium chloride (5%), 17.28g of triethanolamine oleate (0.5%) and stirring uniformly to obtain the high Wen Fanggou corrosion inhibitor B2.
Example 3:
(1) 71.08g of acrylamide (1 mol), 122.10g of propenyl sulfonic acid (1 mol), 98.06g of maleic anhydride (1 mol) and 130.08g of itaconic acid, and 2106.6g of distilled water were added to a reaction vessel, stirring was started and nitrogen was continuously introduced;
(2) 568.64g of Acrylic Acid (AA) (8 times) and 21.32g of hydrogen peroxide (30 percent) are respectively contained in two high-level drip tanks;
(3) after the nitrogen is introduced into the reaction vessel for more than 15 minutes, 24.88g of sodium hypophosphite (35%) is added into the reaction vessel;
(4) starting heating, and dripping the acrylic acid and the hydrogen peroxide prepared in the second step after the temperature reaches more than 50 ℃, wherein the temperature is controlled to be not more than 90 ℃;
(5) stopping introducing nitrogen after the dripping is finished, controlling the temperature to be 75 ℃ and reacting for 4 hours;
(6) 83.82g of methylpyridine (0.90 mol) and 10.66g of acetic anhydride (15%) are added in sequence, the temperature is kept at not more than 90 ℃, and 81.16g of formalin (1.00 mol) is added dropwise;
(7) after the dripping is finished, reacting for 4 hours at 90 ℃ to prepare an intermediate A3;
(8) lowering the temperature to normal temperature, adding 829.60g of polyamino polyether methylene Phosphonic Acid (PAPEMP) (25%), 829.60g of polyol phosphonate (PAPE) (25%), 265.47g of dodecyl dimethyl benzyl ammonium chloride (8%), 9.96g of triethanolamine laurate (0.3%), and stirring uniformly to obtain the high Wen Fanggou corrosion inhibitor B3.
Example 4:
(1) 85.10g of methacrylamide (1 mol), 136.10g of butenyl sulfonic acid (1 mol), 98.06g of maleic anhydride (1 mol) and 130.08g of itaconic acid, and 2246.70g of distilled water were added to a reaction vessel, stirring was started and nitrogen gas was continuously introduced;
(2) 765.90g of Acrylic Acid (AA) (9 times) and 29.79g of hydrogen peroxide (35 percent) are respectively contained in two high-level drip tanks;
(3) after the nitrogen is introduced into the reaction vessel for more than 15 minutes, 25.53g of sodium hypophosphite (30 percent) is added into the reaction vessel;
(4) starting heating, and dripping the acrylic acid and the hydrogen peroxide prepared in the second step after the temperature reaches more than 50 ℃, wherein the temperature is controlled to be not more than 90 ℃;
(5) stopping introducing nitrogen after the dripping is finished, controlling the temperature to be 75 ℃ and reacting for 4 hours;
(6) 69.79g of methylimidazole (0.85 mol) and 12.77g of acetic anhydride (15%) are added in sequence, the temperature is kept at 90 ℃ and 85.22g of formalin (1.05 mol) is added dropwise;
(7) after the dripping is finished, reacting for 6 hours at the temperature of 85 ℃ to prepare an intermediate A4;
(8) to the mixture was cooled to room temperature, 1105.51g of polyamino polyether methylene Phosphonic Acid (PAPEMP) (30%), 737.01g of polyol phosphonate (PAPE) (20%), 368.50g of dodecyldimethylbenzyl ammonium chloride (10%), 3.69g of triethanolamine oleate (0.1%) and 3.69g of triethanolamine laurate (0.1%) were added, and the mixture was stirred uniformly to obtain a high Wen Fanggou corrosion inhibitor B4.
Experimental example 5:
anti-fouling Performance test
Experimental raw materials: water quality ph=7.13 for certain south sea oilfield produced water, evaluation mode: evaluation of the Scale inhibitor Performance reference SY/T5673-1993 method for evaluating the performance of an oilfield scale inhibitor. Experimental temperature: 150 ℃, the dosing concentration is: 50mg/L;
the test results are shown in Table 1:
TABLE 1 scale control Performance test results 1
As can be seen from the above examination data, the scale inhibition rates of sodium polyacrylate, sodium polyepoxysuccinate, AA/AMPS copolymer, 2-phospho-1, 2, 4-tricarboxylic acid butane (PBTCA), PAPEMP, PAPE, hydroxyethylidene diphosphonic acid (HEDP), 2-hydroxyphosphonoacetic acid (HPAA), imidazolinium oleate, pyridinium and quinolinium salts were 82.47%, 59.46%, 81.37%, 85.77%, 84.67%, 60.00%, 82.47%, 55.50%, 3.52%, 2.57% and 2.19%, respectively, of the present invention, examples 1,2, 3, 4 and 5 were 92.47%, 90.56%, 92.26% and 92.26%, respectively, which are significantly higher than the scale inhibition rates of the above products.
Experimental example 6:
anti-fouling Performance test
Experimental raw materials: certain Bohai sea oil field stratum water, quality of water pH=8.33 evaluation mode: evaluation of the Scale inhibitor Performance reference SY/T5673-1993 method for evaluating the performance of an oilfield scale inhibitor. Experimental temperature: 130 ℃, the dosing concentration is as follows: 100mg/L;
the test results are shown in Table 2:
TABLE 2 antifouling property test results 2
As can be seen from the above test data, the scale inhibition rates of sodium polyacrylate, sodium polyepoxysuccinate, AA/AMPS copolymer, 2-phospho-1, 2, 4-tricarboxylic acid butane (PBTCA), PAPEMP, PAPE, hydroxyethylidene diphosphonic acid (HEDP), 2-hydroxyphosphonoacetic acid (HPAA), imidazolinium oleate, pyridinium and quinolinium are 22.01%, 4.38%, 18.29%, 50.41%, 57.89%, 43.74%, 47.70%, 14.90%, 0 and 0, respectively, and the scale inhibition rates of the present invention example 1, example 2, example 3, example 4 and example 5 are 81.10%, 83.55%, 83.78% and 83.17%, respectively, which are significantly higher than those of the above products.
Example 7:
experimental medium: water produced in some south China sea oil field
Evaluation mode: dynamic corrosion experiment of 3 liter Hastelloy steel kettle in room;
experimental materials: n80 steel
Experimental temperature: 150 DEG C
Medium flow rate: 1.0m/s
Experimental gas phase composition: 0.2MPaCO 2 +1.5MpaN 2
Test time: indoor experiment for 72 hours
Concentration of the agent: 50mg/L
The test results were as follows:
TABLE 3 indoor dynamic corrosion test results 1
Example 7:
experimental medium: the method for evaluating the formation water of the oil field in the Bohai sea comprises the following steps: dynamic corrosion experiment of 3 liter Hastelloy steel kettle in room; dissolved oxygen meter experimental material: n80 steel
Experimental temperature: 130 DEG C
Medium flow rate: 1.0m/s
Experimental gas phase composition: 0.5MPaCO 2 +5.0MpaN 2
Test time: indoor experiment for 72 hours
Concentration of the agent: 50mg/L
The test results were as follows:
TABLE 4 results of dynamic Corrosion test and dissolved oxygen measurement in room 2
From the detection data, the invention has higher efficient anti-scaling effect and corrosion inhibition effect on high-temperature corrosion in oilfield production water and formation water compared with various commonly used anti-scaling corrosion inhibitors such as polymers, organic phosphines, heterocyclic compounds and the like.
The foregoing has described exemplary embodiments of the invention, it being understood that any simple variations, modifications, or other equivalent arrangements which would not unduly obscure the invention may be made by those skilled in the art without departing from the spirit of the invention.

Claims (6)

1. An oilfield high Wen Fanggou corrosion inhibitor is characterized by being prepared by the following steps:
firstly, adding equimolar alkenyl amide, alkenyl sulfonic acid, maleic anhydride and itaconic acid and distilled water which is 5 times of the total mass of the alkenyl amide, the alkenyl sulfonic acid, the maleic anhydride and the itaconic acid into a reaction container, starting stirring and continuously introducing nitrogen;
step two, respectively accommodating acrylic acid with the mass of 6-10 times of that of the alkenyl amide and hydrogen peroxide with the mass of 25-40% of that of the alkenyl amide in the reaction container into two high-level liquid drop tanks;
step three, after introducing nitrogen into the reaction vessel for more than 15 minutes, adding sodium hypophosphite accounting for 25-40% of the mass of the alkenyl amide into the reaction vessel;
step four, heating is started, and after the temperature reaches more than 50 ℃, acrylic acid and hydrogen peroxide prepared in the step two are added dropwise at the same time, and the temperature is controlled to be not more than 90 ℃;
stopping introducing nitrogen after the dripping is finished, controlling the temperature to be 75-90 ℃ and reacting for 2-4 hours;
sequentially adding methyl nitrogenous heterocyclic compound with the mole ratio of alkenyl amide of 0.8:0.95, wherein the mass of anhydride with the mass of alkenyl amide of 10-20 percent, continuously controlling the temperature to be not more than 90 ℃, and dropwise adding formalin with the mole ratio of alkenyl amide of 1:1.05;
step seven, after the dripping is finished, reacting for 4 to 8 hours at the temperature of 80 to 95 ℃ to prepare an intermediate A;
step eight, reducing to normal temperature, adding one or two of polyamino polyether methylene phosphonic acid accounting for 20-30% of the total mass of the intermediate A, polyol phosphonate accounting for 20-30% of the total mass of the intermediate A, dodecyl dimethyl benzyl ammonium chloride accounting for 5-10% of the total mass of the intermediate A, triethanolamine benzoate, triethanolamine oleate and triethanolamine laurate accounting for 0.1-0.5% of the total mass of the intermediate A, and uniformly stirring to obtain the high Wen Fanggou corrosion inhibitor;
wherein the methyl nitrogen-containing heterocyclic compound is picoline, methylquinoline or methylimidazole.
2. An oilfield high Wen Fanggou corrosion inhibitor according to claim 1, wherein: the alkenyl amide is acrylamide or methacrylamide.
3. An oilfield high Wen Fanggou corrosion inhibitor according to claim 1, wherein: the alkenyl sulfonic acid is vinyl sulfonic acid, allyl sulfonic acid, propenyl sulfonic acid or butenyl sulfonic acid.
4. An oilfield high Wen Fanggou corrosion inhibitor according to claim 1, wherein: the anhydride is formic anhydride, acetic anhydride or propionic anhydride.
5. A preparation method of an oilfield high Wen Fanggou corrosion inhibitor is characterized by comprising the following steps: the method comprises the following steps of:
firstly, adding equimolar alkenyl amide, alkenyl sulfonic acid, maleic anhydride and itaconic acid and distilled water which is 5 times of the total mass of the alkenyl amide, the alkenyl sulfonic acid, the maleic anhydride and the itaconic acid into a reaction container, starting stirring and continuously introducing nitrogen;
step two, respectively accommodating acrylic acid with the mass of 6-10 times of that of the alkenyl amide and hydrogen peroxide with the mass of 25-40% of that of the alkenyl amide in the reaction container into two high-level liquid drop tanks;
step three, after introducing nitrogen into the reaction vessel for more than 15 minutes, adding sodium hypophosphite accounting for 25-40% of the mass of the alkenyl amide into the reaction vessel;
step four, heating is started, and after the temperature reaches more than 50 ℃, acrylic acid and hydrogen peroxide prepared in the step two are added dropwise at the same time, and the temperature is controlled to be not more than 90 ℃;
stopping introducing nitrogen after the dripping is finished, controlling the temperature to be 75-90 ℃ and reacting for 2-4 hours;
sequentially adding methyl nitrogenous heterocyclic compound with the mole ratio of alkenyl amide of 0.80:0.95, adding anhydride with the mass of 10-20% of that of alkenyl amide, continuously controlling the temperature to be not more than 90 ℃, and dropwise adding formalin with the mole ratio of alkenyl amide of 1:1.05;
step seven, after the dripping is finished, reacting for 4 to 8 hours at the temperature of 80 to 95 ℃ to prepare an intermediate A;
step eight, reducing to normal temperature, adding one or two of polyamino polyether methylene phosphonic acid accounting for 20-30% of the total mass of the intermediate A, polyol phosphonate accounting for 20-30% of the total mass of the intermediate A, dodecyl dimethyl benzyl ammonium chloride accounting for 5-10% of the total mass of the intermediate A, triethanolamine benzoate, triethanolamine oleate and triethanolamine laurate accounting for 0.1-0.5% of the total mass of the intermediate A, and uniformly stirring to obtain the high Wen Fanggou corrosion inhibitor;
wherein the methyl nitrogen-containing heterocyclic compound is picoline, methylquinoline or methylimidazole; the anhydride is formic anhydride, acetic anhydride or propionic anhydride.
6. The method for preparing the oilfield high Wen Fanggou corrosion inhibitor according to claim 5, wherein the method comprises the following steps: the alkenyl amide is acrylamide and methacrylamide; the alkenyl sulfonic acid is vinyl sulfonic acid, allyl sulfonic acid, propenyl sulfonic acid or butenyl sulfonic acid.
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