CN105419774A - Preparation method of acidizing corrosion inhibitor in high-temperature and concentrated acid environment - Google Patents
Preparation method of acidizing corrosion inhibitor in high-temperature and concentrated acid environment Download PDFInfo
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Abstract
The invention relates to a preparation method of acidizing corrosion inhibitor in a high-temperature and concentrated acid environment. The preparation method is used for an acidification technology in carbonate oil reservoir exploration and overcomes the problem that existing high-temperature acidification corrosion inhibitor is poor in solubility and dispersion in use and prone to coking. According to the technical scheme, firstly, formaldehyde, benzene methanamine, absolute ethyl alcohol and concentrated hydrochloric acid are added into a three-necked flask, and then the three-necked flask is placed into an oil bath pan with the temperature being 110 DEG C for conducting a reaction for 2 hours; then, acetophenone is added, the pH is adjusted to 4 through concentrated hydrochloric acid, a reaction is conducted for 4 hours, and a coarse mannich base is obtained; thirdly, a vacuum rotary evaporation instrument is utilized for purification, separation is conducted, and a mannich base intermediate is obtained; fourthly, after the intermediate obtained in step 3 is washed, benzyl chloride is added, a reaction is conducted for 6 hours at the temperature of 110 DEG C, evaporation and separation are conducted through the vacuum rotary evaporation instrument, and mannich base quaternary ammonium salt is obtained; finally, potassium iodide is added in the mannich base quaternary ammonium salt stirring process for conducting mixed distribution, and the high-temperature acidizing corrosion inhibitor is obtained. The acidizing corrosion inhibitor has good solubility and dispersion, can further improve corrosion inhibition efficiency and is good in stability.
Description
Technical field
The invention belongs to oil production chemical field, relate to a kind of preparation method for the acidification corrosion inhibitor in high temperature concentrated acid environment for the acidification technique in carbonate oil reservoir development process.
Technical background
In the performance history of petroleum and natural gas, the normal object adopting Acidizing Technology to reach volume increase.In acidizing treatment process, the injection of acid will cause surperficial pitting corrosion, the hydrogen-induced cracking even brittle rupture of Oil/gas Well tubing and underground equipment, sometimes also may cause the sudden break accident of downhole tubular goods, cause serious financial loss; Also formation may cause possible permanent damage with the metallic iron ion of acid-respons simultaneously.When carrying out the larger deep-well acidifying of acid amount for high temperature deep well, ultra deep well, the Anticorrosion of oil pipe and equipment must be considered.The use of acidification corrosion inhibitor is simple, less investment and can effectively suppress acid solution to the corrosion of tubing and casing and equipment, is the important method solving etching problem in acidizing treatment engineering.At present, develop of a great variety and widely used corrosion inhibitor product both at home and abroad, but the shortcomings such as the at high temperature easy coking of ubiquity of domestic high-temperature acidification corrosion inhibitor, layering, the dispersed instability of solvability.With the Mannich alkaline inhibiter that aldehyde, ketone, amine obtain for Material synthesis, organic compound molecule amount is little, containing multiple nitrogen-atoms with lone-pair electron or Sauerstoffatom in molecule, secondly Mannich base molecule itself is a chelating ligand,, there is complexing action, and there is good solubility in acid in easy formation coordinate bond, and high temperature resistant, resistance to concentrated acids can be good, thus can keep stronger suitability to high temperature oil.
Summary of the invention
Object of the present invention: in order to overcome existing high-temperature acidification corrosion inhibitor in use solvability, dispersiveness is not good, the problem of easy coking, for improving the resistance to elevated temperatures of acidification corrosion inhibitor, spy provides a kind of preparation method for the acidification corrosion inhibitor in high temperature concentrated acid environment.
In order to achieve the above object, by the following technical solutions, a kind of preparation method for the acidification corrosion inhibitor in high temperature concentrated acid environment: first utilize Mannich reaction, synthesizes and a kind ofly can be applicable to high temperature acidified Mannich base intermediate in the present invention; Then further Mannich base intermediate is carried out quaterisation, strengthen solvability and the dispersiveness of inhibiter; Finally add iodide ion auxiliary agent, produce synergistic function with Mannich base quaternary ammonium salt system, there is excellent corrosion mitigating effect, resistance to elevated temperatures, and stable memory property.
Preparation method of the present invention comprise " two-step approach " synthesizing mannich alkali intermediate, Mannich base quaternary ammonium salt synthesis and formula modulation composite three steps:
The first step " two-step approach " synthesizing mannich alkali intermediate:
(1) with formaldehyde, benzene methanamine, methyl phenyl ketone is raw material, solvent made by dehydrated alcohol, concentrated hydrochloric acid makes catalyzer, raw materials used mol ratio is: formaldehyde: benzene methanamine: methyl phenyl ketone=1 ~ 1.2:1 ~ 1.2:1, first with thermometer, in the three-necked flask of serpentine condenser and agitator, add formaldehyde 7.20g (molar mass 30, amount of substance 0.24), benzene methanamine 25.68g (molar mass 107, amount of substance 0.235), add 20ml dehydrated alcohol again, 6ml concentrated hydrochloric acid, three-necked flask is put into the oil bath pan that temperature of reaction is 110 DEG C, under agitation the reaction times is 2h,
(2) then add methyl phenyl ketone 24.00g (molar mass 108, amount of substance 0.22), slowly drip concentrated hydrochloric acid adjust ph to 4, under above-mentioned uniform temp He under stir speed (S.S.), react 4h, obtained rough Mannich base intermediate;
(3) finally with vacuum rotary evaporator, product is purified, rotary distillation temperature is 85 DEG C, rotating speed 60r/min, Vacuum Pressure-0.09MPa, rotary distillation end mark is that bubble-free is emerged, pour product of distillation into separating funnel, after leaving standstill 20 ~ 30min, be separated and obtain Mannich base intermediate.Chemical equation is:
The synthesis of second step Mannich base quaternary ammonium salt:
(1) after the Mannich base intermediate anhydrous ethanol solvent washing the first step obtained, add Benzyl Chloride 10.12g (molar mass 126.5, amount of substance 0.08), Mannich base intermediate 23.90g (molar mass 239, amount of substance 0.1), 6h is reacted at temperature is 110 DEG C, raw materials used mol ratio: Mannich base intermediate: Benzyl Chloride=1:1 ~ 0.8
(2) then evaporate with vacuum rotary evaporator, rotary distillation temperature is 85 DEG C, and rotating speed is 60r/min, and Vacuum Pressure is rotary evaporation under the condition of-0.09MPa, finally product of distillation is left standstill 20min in separating funnel, isolate upper part and namely obtain Mannich base quaternary ammonium salt.Chemical equation is:
3rd step formula modulation is composite: the Mannich base quaternary ammonium salt 2377.6mg that on adding in three-necked flask, step synthesis is obtained, adds 173.2mgKI and mixes composite, obtain high-temperature acidification corrosion inhibitor product in whipping process.
The invention has the beneficial effects as follows: (1) adopts benzene methanamine, methyl phenyl ketone, formaldehyde to be synthesis material, by " two-step synthesis method " synthesizing mannich alkali intermediate, not only decrease the generation of side reaction, and " one kettle way " that difference is conventional, corrosion mitigating effect is more excellent; (2) obtained Mannich base quaternary ammonium salt high-temperature acidification corrosion inhibitor proves through test, and have good resistance to elevated temperatures, noncoking under the acidulated condition of 120 DEG C ~ 150 DEG C, can be applicable to acidizing treatment; (3) this acidification corrosion inhibitor has good solvability and dispersiveness, and stablizes not stratified, after adding iodide ion additive compound, can further improve its inhibition efficiency, and under 20% hydrochloric acid acidic conditions, corrosion inhibition rate is all greater than 90%.
Embodiment
Example 1: a kind of preparation for the acidification corrosion inhibitor in high temperature concentrated acid environment, dissolution dispersity and storge quality measure, and its concrete steps are as follows:
The first step " two-step approach " synthesizing mannich alkali intermediate, with formaldehyde, benzene methanamine, methyl phenyl ketone for raw material, wherein the mol ratio of raw material monomer used is: formaldehyde: benzene methanamine: methyl phenyl ketone=1 ~ 1.2:1 ~ 1.2:1.First add formaldehyde 7.20g, benzene methanamine 25.68g, solvent made by 20ml dehydrated alcohol, 6ml concentrated hydrochloric acid makes catalyzer, react in the three-necked flask that thermometer, serpentine condenser and agitator be housed and in the oil bath pan of 110 DEG C, reaction times is 2h, then adds methyl phenyl ketone 24.00g, slowly drips concentrated hydrochloric acid regulation system pH value to 4, react 4h at the same temperature with under stir speed (S.S.), obtain rough Mannich base intermediate.Purify to Mannich base intermediate with vacuum rotary evaporator subsequently, rotary distillation temperature is 85 DEG C, rotating speed 60r/min, Vacuum Pressure-0.09MPa, rotary distillation end mark is that bubble-free is emerged, and after product leaves standstill 25min, is separated obtains Mannich base intermediate with separating funnel.
The synthesis of second step Mannich base quaternary ammonium salt: after the Mannich base intermediate anhydrous ethanol solvent washing that the first step is obtained, with material molar ratio: Mannich base intermediate: the ratio of Benzyl Chloride=1:1 ~ 0.8, add Mannich base intermediate 23.90g, Benzyl Chloride 10.12g, be contained in serpentine condenser, in the three-necked flask of agitator and thermometer, 6h is reacted at 110 DEG C, by vacuum rotary evaporator at 85 DEG C, rotating speed 60r/min, rotary evaporation under the condition of Vacuum Pressure-0.09MPa, finally in separating funnel, leave standstill 20min, isolate upper part and namely obtain Mannich base quaternary ammonium salt.
3rd step formula modulation is composite: get step and synthesize the Mannich base quaternary ammonium salt 2377.6mg obtained and stir, add the KI of 173.2mg in whipping process, acquisition high-temperature acidification corrosion inhibitor product.
(1) dissolution dispersity measures: pour in colorimetric cylinder by the hydrochloric acid 100ml of 20% concentration prepared, then in colorimetric cylinder, the Mannich base quaternary ammonium salt corrosion inhibitor of 3% is added with transfer pipet, cover under putting into 50 DEG C of thermostat water bath water bath with thermostatic control horizontal planes after bottle cap shakes up and measure dissolution dispersity, observe in 48h acid solution keep evenly, without layering, not precipitation.
(2) storge quality measures: the high-temperature acidification corrosion inhibitor of preparation is stored 15 days at-5 DEG C and 25 DEG C, finds that inhibiter is still even, does not have layering.By static weight loss method at 130 DEG C, hydrochloric acid mass percentage concentration is that to add concentration under the condition of 20% be acidification corrosion inhibitor after the storage of 0.5%, and lacing film steel is P110 level casing steel, carries out corrosion coupon experiment, and recording its inhibition efficiency is 99.4%.
Example 2: a kind of preparation method for the acidification corrosion inhibitor in high temperature concentrated acid environment and corrosion inhibition measure, and its concrete steps are as follows:
The first step " two-step approach " synthesizing mannich alkali intermediate: with formaldehyde, benzene methanamine, methyl phenyl ketone for raw material, wherein the mol ratio of raw material monomer used is: formaldehyde: benzene methanamine: methyl phenyl ketone=1 ~ 1.2:1 ~ 1.2:1.First add formaldehyde 6.90g, benzene methanamine 24.61g, solvent made by 20ml dehydrated alcohol, 6ml concentrated hydrochloric acid makes catalyzer, react in the three-necked flask that thermometer, serpentine condenser and agitator be housed and in the oil bath pan of 110 DEG C, reaction times is 2h, then adds methyl phenyl ketone 24.00g, slowly drips concentrated hydrochloric acid regulation system pH value to 4, react 4h at the same temperature with under stir speed (S.S.), obtain rough Mannich base intermediate.Purify to Mannich base intermediate with vacuum rotary evaporator subsequently, rotary distillation temperature is 85 DEG C, rotating speed 60r/min, Vacuum Pressure-0.09MPa, rotary distillation end mark is that bubble-free is emerged, and after product leaves standstill 25min, is separated obtains Mannich base intermediate with separating funnel.
The synthesis of second step Mannich base quaternary ammonium salt: after the Mannich base intermediate anhydrous ethanol solvent washing that the first step is obtained, with material molar ratio: Mannich base intermediate: Benzyl Chloride=1:1 ~ 0.8, add Mannich base intermediate 23.90g, Benzyl Chloride 11.38g, be contained in serpentine condenser, in the three-necked flask of agitator and thermometer, 6h is reacted at 110 DEG C, by vacuum rotary evaporator at 85 DEG C, rotating speed 60r/min, rotary evaporation under the condition of Vacuum Pressure-0.09MPa, finally in separating funnel, leave standstill 20min, isolate upper part and be required Mannich base quaternary ammonium salt.
3rd step formula modulation is composite: get the Mannich base quaternary ammonium salt 2377.6mg synthetic product that step obtains and stir, add the KI of 173.2mg in whipping process, obtain high-temperature acidification corrosion inhibitor product.
(1) static weight loss method: the P110 sample selecting 30mm × 15mm × 3mm, specimen surface is polished smooth, respectively with W28 and W14 abrasive paper for metallograph corase grind removing specimen surface corrosion product and burr, smooth to its smooth surface with the test piece of W10, W07 and W05 abrasive paper for metallograph fine grinding again, then by precision be the size of the vernier caliper measurement sample of 0.02mm and record.Then test piece is successively put into acetone and dehydrated alcohol immersion also sonic oscillation cleaning 5min, oil removing is carried out to specimen surface and dewaters, and with absorbent cotton wiping specimen surface, then sample cold wind is dried up, weigh with electronic balance (precision is 0.1mg) after putting into the dry 20min of moisture eliminator.
Cotton thread dry for corrosion sample is hung the three-necked flask putting into 500ml, every three are one group and do parallel sample, during experiment, HCl solution used all adopts now with the current, configuration 470ml acid solution, gets the Mannich base inhibiter of different content, stirs with glass stick, then pour into and hung up properly in the three-necked flask of sample, connect serpentine condenser, three-necked flask is put into heated up complete water-bath or oil bath pan, after leaving standstill corrosion 4h, take out test piece.
Corrosion sample falls the hydrochloric acid solution of remained on surface immediately with tap water after taking out, before membrane removal, put into acetone soak 5min and the loose product removing surface with scrub-brush, then put into membrane removal liquid and soak 5min, then to dewater further oil removing with rayon balls wiping strip with acetone, dehydrated alcohol, finally dry up with cold wind and weigh with electronic balance (precision is 0.1mg) after putting into the dry 20min of moisture eliminator.
At 130 DEG C, in under 30% hcl corrosion environment, utilize static weight loss method to obtain, under the inhibiter dosage of 0.1% ~ 2%, all reach more than 98% to the inhibition efficiency of P110 level casing steel corrosion coupon, its corrosion mitigating effect all reaches two-level index level in SY/T5405-1996 standard.
(2) method of polarization curve: electro-chemical test working electrode is P110 steel, test piece is processed into the square of 1cm × 1cm, is welded by copper cash with test piece, then only reserves to be tested with epoxy sealing.Before test, by sample testing face polishing (polishing process is consistent with static weight loss method) to smooth, then respectively with being moistened with the absorbent cotton wiping of alcohol and acetone with the oil removing that dewaters to test piece, then cold wind dries up stand-by.
Experiment test temperature is 30 DEG C, and corrosive medium is 20% hydrochloric acid soln.Polarization curve test parameter is: scanning speed is 1mV/s, and sweep limit is corrosion potential ± 400mV, adds 0% respectively, 0.1%, 0.5%, 1%, the Mannich base quaternary ammonium salt corrosion inhibitor of 1.5%, 2%, carries out polarization curve test, result matching obtains inhibition efficiency and is respectively 0,99.63%, 99.82%, 99.72%, 99.96%, 99.95%.
(3) AC impedence method: experiment test temperature is 30 DEG C, corrosive medium is 20% hydrochloric acid soln.Ac impedance measurement parameter: alternating-current amplitude ± 10mvvs.O.C (corrosion potential), test frequency scope 10mHz-10kHz, add the Mannich base quaternary ammonium salt corrosion inhibitor that massfraction is 0.1%, 0.5%, 1%, 1.5% and 2% respectively, it is 0% that result matching obtains inhibition efficiency, 89.84%, 90.86%, 91.72%, 92.69%, 93.98%.
Example 3: a kind of preparation method for the acidification corrosion inhibitor in high temperature concentrated acid environment and morphology observation, its concrete steps are as follows:
The first step " two-step approach " synthesizing mannich alkali intermediate: with formaldehyde, benzene methanamine, methyl phenyl ketone for raw material, the wherein mol ratio of raw material monomer used: formaldehyde: benzene methanamine: methyl phenyl ketone=1 ~ 1.2:1 ~ 1.2:1.First add formaldehyde 6.00g, benzene methanamine 21.40g, solvent made by 20ml dehydrated alcohol, 6ml concentrated hydrochloric acid makes catalyzer, react in the three-necked flask that thermometer, serpentine condenser and agitator be housed and in the oil bath pan of 110 DEG C, reaction times is 2h, then adds methyl phenyl ketone 24.00g, slowly drips concentrated hydrochloric acid and regulates pH value in reaction to 4, react 4h at the same temperature with under stir speed (S.S.), obtain rough Mannich base intermediate.Purify to Mannich base intermediate with vacuum rotary evaporator subsequently, rotary distillation temperature is 85 DEG C, rotating speed 60r/min, Vacuum Pressure-0.09MPa, rotary distillation end mark is that bubble-free is emerged, and after product leaves standstill 20 ~ 30min, is separated obtains Mannich base intermediate with separating funnel.
The synthesis of second step Mannich base quaternary ammonium salt: after the Mannich base intermediate anhydrous ethanol solvent washing that the first step is obtained, with material molar ratio: Mannich base intermediate: Benzyl Chloride=1:1 ~ 0.8, add Mannich base intermediate 23.90g, Benzyl Chloride 12.65g, be contained in serpentine condenser, in the three-necked flask of agitator and thermometer, 4h is reacted at 90 DEG C, by vacuum rotary evaporator at 85 DEG C, rotating speed 60r/min, rotary evaporation under the condition of Vacuum Pressure-0.09MPa, finally in separating funnel, leave standstill 20min, isolate upper part and be required Mannich base quaternary ammonium salt.
3rd step formula modulation is composite: above walk the Mannich base quaternary ammonium salt 2377.6mg synthetic product obtained and stir, add the KI of 173.2mg in whipping process, obtain high-temperature acidification corrosion inhibitor product.
The film forming microscopic appearance carrying out inhibiter under laboratory is observed: P110 steel disc is at 130 DEG C, and concentration of hydrochloric acid solution is corrode 4h under 20% condition, and adding density of corrosion inhibitor is that 1%, SEM observes that steel disc surface forms the effective protective membrane of one deck.
Claims (1)
1. the preparation method for the acidification corrosion inhibitor in high temperature concentrated acid environment, it is characterized in that: this acidification corrosion inhibitor is by Mannich base quaternary ammonium salt and the composite gained of potassiumiodide, its preparation method comprises three steps: the first step synthesizing mannich alkali intermediate, with formaldehyde, benzene methanamine, methyl phenyl ketone for raw material, solvent made by dehydrated alcohol, concentrated hydrochloric acid makes catalyzer, and raw materials used mol ratio is: formaldehyde: benzene methanamine: methyl phenyl ketone=1 ~ 1.2:1 ~ 1.2:1; First in the three-necked flask with thermometer, serpentine condenser and agitator, add formaldehyde 7.20g, benzene methanamine 25.68g, add 20ml dehydrated alcohol, 6ml concentrated hydrochloric acid again, three-necked flask being put into temperature is that the oil bath pan of 110 DEG C reacts, and under agitation the reaction times is 2h; Then add methyl phenyl ketone 24.00g, slowly drip concentrated hydrochloric acid regulation system pH value to 4, under said temperature and stir speed (S.S.), react 4h, obtained rough Mannich base intermediate; Finally purify to raw product with vacuum rotary evaporator, rotary distillation temperature is 85 DEG C, rotating speed 60r/min, Vacuum Pressure-0.09MPa, distillation of stopping the rotation when bubble-free is emerged, pours product of distillation into separating funnel, after leaving standstill 20 ~ 30min, be separated and obtain Mannich base intermediate; The synthesis of second step Mannich base quaternary ammonium salt, after the Mannich base intermediate absolute ethanol washing that upper step is obtained, mol ratio by raw material: Mannich base intermediate: the ratio of Benzyl Chloride=1:1 ~ 0.8 adds Mannich base intermediate 23.90g and 10.12g Benzyl Chloride, load in three-necked flask, at temperature is 110 DEG C, reacts 6h; Then vacuum rotary evaporator rotary evaporation is used, rotary distillation temperature is 85 DEG C, and rotating speed is 60r/min, rotary evaporation under the condition of Vacuum Pressure-0.09MPa, finally product of distillation is left standstill 20min in separating funnel, isolate upper part and namely obtain Mannich base quaternary ammonium salt; 3rd step formula modulation is composite, adds the 2377.6mg Mannich base quaternary ammonium salt that synthesis is obtained in three-necked flask, adds 173.2mg potassiumiodide and mix composite in whipping process, obtained this high-temperature acidification corrosion inhibitor product.
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