CN104910028A - Preparation method and application of aldehyde ketone amine condensate corrosion inhibitor for acidification - Google Patents
Preparation method and application of aldehyde ketone amine condensate corrosion inhibitor for acidification Download PDFInfo
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- CN104910028A CN104910028A CN201510397228.3A CN201510397228A CN104910028A CN 104910028 A CN104910028 A CN 104910028A CN 201510397228 A CN201510397228 A CN 201510397228A CN 104910028 A CN104910028 A CN 104910028A
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- inhibiter
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- aldehyde ketone
- ketone amine
- hydrochloric acid
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Abstract
The invention relates to a preparation method and application of an aldehyde ketone amine condensate corrosion inhibitor for acidification, and aims to solve the problem that concentrated acid corrodes equipment when acidification is performed during yield increase of an oil-gas well. According to the technical scheme, the preparation method comprises the following steps: firstly, cyclohexylamine with a molar ratio of 1-2 is dissolved in 10 ml of 1, 4-dioxane solvent, is moved into a three-necked flask which is fed with nitrogen for protection, and is heated up to 60-90 DEG C; then, cinnamaldehyde with a molar ratio of 1-1.4 and benzalacetone with a molar ratio of 1 are added to react at 60-90 DEG C for 5-9 hours so as to obtain a product; finally, the product is moved into a vacuum rotary evaporator and is subjected to vacuum distillation at 90 DEG C so as to obtain the aldehyde ketone amine condensate corrosion inhibitor. According to the preparation method, the prepared corrosion inhibitor is added to concentrated hydrochloric acid, steel is immersed and subjected to the immersion test, and the results show that the corrosion rate is 3.14-4.75 g/(m2.h) and the corrosion inhibition rate is 99.91%-99.94%, which reaches the standard of first-grade products in this industry. The preparation method is simple and needs no special equipment; the aldehyde ketone amine condensate corrosion inhibitor is used in the acidification operation of a concentrated hydrochloric acid or mud acid oil-gas well.
Description
Technical field
The present invention relates to a kind of preparation method for acidifying aldehyde ketone amine condenses inhibiter in well production increment operation use and application thereof.
Background technology
Acidifying is one of effective technology measure of well production increment, water injection well stimulation in the oil reservoir development process of petroleum industry field.Although improve the rate of oil and gas recovery, also easily cause the corrosion of oil pipe and down-hole hardware simultaneously, also likely cause the sudden of tubing to be broken, cause very large financial loss.
Along with the development of drilling technology and the progress of oil recovery technique, the exploitation of a large amount of profound level infiltration oil reservoirs, the acidifying of high temperature concentrated acid increases year by year, and solving the corrosion of concentrated acid liquid to equipment is one of problem demanding prompt solution on current oil field.Amino acids, imidazolines, alkynol class, quaternary ammonium salt, Schiff bases, Mannich bases, thiazoles, polymer class, mineral-type etc. are mainly contained at present for concentrated acid acidification corrosion inhibitor.The acidification corrosion inhibitor of current use acid-soluble poor, formation has injury, and addition is comparatively large, and easily occur precipitation when temperature is higher, corrosion inhibition rate is lower.So research and development is used for high concentrated acid, Low Damage, high efficiency inhibiter are one of significant task facing of oil worker.
Summary of the invention
The object of the invention is: during in order to solve acidifying in well production increment, concentrated acid is to the corrosion of equipment, overcome the acid-soluble poor of the acidification corrosion inhibitor used at present, formation has injury, addition is larger, there is precipitation, the problems such as corrosion inhibition rate is lower, spy provides a kind of preparation method and application of acidifying aldehyde ketone amine condenses inhibiter.
For solving the problem, the present invention is by the following technical solutions: a kind of preparation method of acidifying aldehyde ketone amine condenses inhibiter, comprises the following steps: the amount of substance mol ratio preparing this inhibiter raw materials used is: benzylideneacetone: hexahydroaniline: phenylacrolein=1: 1 ~ 2: 1 ~ 1.4; By mol ratio be first 1 ~ 2 hexahydroaniline be dissolved in 10ml1, in 4-dioxane solvent, move in there-necked flask and pass into nitrogen protection, be warming up to 60 ~ 90 DEG C; Then add successively mol ratio be 1 ~ 1.4 phenylacrolein and mol ratio be the benzylideneacetone of 1, at temperature is 60 ~ 90 DEG C react 5 ~ 9h; Finally product is moved in vacuum rotary evaporator, at 90 DEG C, carry out underpressure distillation obtain this aldehyde ketone amine condenses inhibiter.
The application of aldehyde ketone amine condenses in acid solution inhibition prepared by above-mentioned preparation method, it is the aldehyde ketone amine condenses inhibiter of 0.8% of acid solution total amount by quality, joining massfraction concentration is in the concentrated hydrochloric acid of 20%, being hung by A3 steel disc immerses in above-mentioned hydrochloric acid soln, at temperature is 90 DEG C, soaks 4h, then takes out, cleaning, dry, weigh; Through experiment detection display, the erosion rate of A3 steel disc is 3.14 ~ 4.75g/ (m
2h), corrosion inhibition rate is 99.91% ~ 99.94%; According to standard SY/T 5405-1996 first grade require regulation, at 90 DEG C 20% concentrated hydrochloric acid in corrosion speed be 3 ~ 5g/ (m
2h).Prove that this inhibiter has reached first grade required standard by experiment.
The present invention compared with the prior art, has following beneficial effect: (1) this preparation method technique is simple, without the need to specific installation, reduces production cost; (2) inhibiter that obtains of this preparation method, corrosion inhibition rate >99.90%, good dispersity in hydrochloric acid and mud acid solution, have good surfactivity, coking is few, and in high temperature acidified liquid, erosion rate reaches the primary standard of industry; (3) this aldehyde ketone amine condenses inhibiter Applicable temperature is at 90 DEG C, concentration be 15% ~ 20% concentrated hydrochloric acid or mud acid well production increment construction operation in.
Embodiment
Embodiment 1
First will take 4.96g hexahydroaniline and be dissolved in 10ml1, and in 4-dioxane solvent, move in there-necked flask and pass into nitrogen protection, be warming up to 60 DEG C; Then 6.61g phenylacrolein and 7.31g benzylideneacetone is dripped successively, reaction 8h; Finally product is moved in vacuum rotary evaporator, at 90 DEG C, carry out underpressure distillation obtain this aldehyde ketone amine condenses inhibiter.
Carry out corrosion inhibition evaluation by the aldehyde ketone amine condenses inhibiter of static weight loss method to synthesis, it is in the concentrated hydrochloric acid of 20% that this inhibiter of 4.5g is added massfraction, is hung by A3 steel disc and immerses in above-mentioned hydrochloric acid soln, at temperature is 90 DEG C, soaks 4h, then takes out, cleaning, dry, weigh; Through experiment detection display, the erosion rate of A3 steel disc is 4.75g/m
2* h, corrosion inhibition rate is 99.91%; According to standard SY/T 5405-1996 first grade require regulation, at 90 DEG C 20% concentrated hydrochloric acid in corrosion speed be 3 ~ 5g/ (m
2h).Prove that this inhibiter has reached first grade required standard by experiment.
Embodiment 2
First will take 4.96g hexahydroaniline and be dissolved in 10ml1, and in 4-dioxane solvent, move in there-necked flask and pass into nitrogen protection, be warming up to 70 DEG C; Then 8.60g phenylacrolein and 7.31g benzylideneacetone is dripped successively, reaction 7h; Finally product is moved in vacuum rotary evaporator, at 90 DEG C, carry out underpressure distillation obtain this aldehyde ketone amine condenses inhibiter.
Carry out corrosion inhibition evaluation by the aldehyde ketone amine condenses inhibiter of static weight loss method to synthesis, it is in the concentrated hydrochloric acid of 20% that this inhibiter of 4.5g is added massfraction, is hung by A3 steel disc and immerses in above-mentioned hydrochloric acid soln, at temperature is 90 DEG C, soaks 4h, then takes out, cleaning, dry, weigh; Through experiment detection display, the erosion rate of A3 steel disc is 3.46g/m
2* h, corrosion inhibition rate is 99.93%; According to standard SY/T 5405-1996 first grade require regulation, at 90 DEG C 20% concentrated hydrochloric acid in corrosion speed be 3 ~ 5g/ (m
2h).Prove that this inhibiter has reached first grade required standard by experiment.
Embodiment 3
First will take 7.44g hexahydroaniline and be dissolved in 10ml1, and in 4-dioxane solvent, move in there-necked flask and pass into nitrogen protection, be warming up to 70 DEG C; Then 7.27g phenylacrolein and 7.31g benzylideneacetone is dripped successively, reaction 6h; Finally product is moved in vacuum rotary evaporator, at 90 DEG C, carry out underpressure distillation obtain this aldehyde ketone amine condenses inhibiter.
Carry out corrosion inhibition evaluation by the aldehyde ketone amine condenses inhibiter of static weight loss method to synthesis, it is in the concentrated hydrochloric acid of 20% that this inhibiter of 4.5g is added massfraction, is hung by A3 steel disc and immerses in above-mentioned hydrochloric acid soln, at temperature is 90 DEG C, soaks 4h, then takes out, cleaning, dry, weigh; Through experiment detection display, the erosion rate of A3 steel disc is 3.14g/m
2* h, corrosion inhibition rate is 99.94%; According to standard SY/T 5405-1996 first grade require regulation, at 90 DEG C 20% concentrated hydrochloric acid in corrosion speed be 3 ~ 5g/ (m
2h).Prove that this inhibiter has reached first grade required standard by experiment.
Embodiment 4
First will take 7.44g hexahydroaniline and be dissolved in 10ml1, and in 4-dioxane solvent, move in there-necked flask and pass into nitrogen protection, be warming up to 80 DEG C; Then 6.61g phenylacrolein and 7.31g benzylideneacetone is dripped successively, reaction 9h; Finally product is moved in vacuum rotary evaporator, at 90 DEG C, carry out underpressure distillation obtain this aldehyde ketone amine condenses inhibiter.
Carry out corrosion inhibition evaluation by the aldehyde ketone amine condenses inhibiter of static weight loss method to synthesis, it is in the concentrated hydrochloric acid of 20% that this inhibiter of 4.5g is added massfraction, is hung by A3 steel disc and immerses in above-mentioned hydrochloric acid soln, at temperature is 90 DEG C, soaks 4h, then takes out, cleaning, dry, weigh; Through experiment detection display, the erosion rate of A3 steel disc is 3.52g/m
2* h, corrosion inhibition rate is 99.93%; According to standard SY/T 5405-1996 first grade require regulation, at 90 DEG C 20% concentrated hydrochloric acid in corrosion speed be 3 ~ 5g/ (m
2h).Prove that this inhibiter has reached first grade required standard by experiment.
Embodiment 5
First will take 7.44g hexahydroaniline and be dissolved in 10ml1, and in 4-dioxane solvent, move in there-necked flask and pass into nitrogen protection, be warming up to 70 DEG C; Then 9.60g phenylacrolein and 7.31g benzylideneacetone is dripped successively, reaction 9h; Finally product is moved in vacuum rotary evaporator, at 90 DEG C, carry out underpressure distillation obtain this aldehyde ketone amine condenses inhibiter.
Carry out corrosion inhibition evaluation by the aldehyde ketone amine condenses inhibiter of static weight loss method to synthesis, it is in the concentrated hydrochloric acid of 20% that this inhibiter of 4.5g is added massfraction, is hung by A3 steel disc and immerses in above-mentioned hydrochloric acid soln, at temperature is 90 DEG C, soaks 4h, then takes out, cleaning, dry, weigh; Through experiment detection display, the erosion rate of A3 steel disc is 4.45g/m
2* h, corrosion inhibition rate is 99.92%; According to standard SY/T 5405-1996 first grade require regulation, at 90 DEG C 20% concentrated hydrochloric acid in corrosion speed be 3 ~ 5g/ (m
2h).Prove that this inhibiter has reached first grade required standard by experiment.
Can be drawn by above embodiment, preparation method's technique of this aldehyde ketone amine condenses inhibiter is simple, without the need to specific installation; At being applicable to 90 DEG C in 15% ~ 20% concentrated hydrochloric acid or the job execution of soil acid acidizing well production increment, corrosion inhibition rate >99.90%.
Claims (2)
1. an acidifying preparation method for aldehyde ketone amine condenses inhibiter, is characterized in that: the amount of substance mol ratio preparing this inhibiter raw materials used is: benzylideneacetone: hexahydroaniline: phenylacrolein=1: 1 ~ 2: 1 ~ 1.4; By mol ratio be first 1 ~ 2 hexahydroaniline be dissolved in 10ml Isosorbide-5-Nitrae-dioxane solvent, move in there-necked flask and pass into nitrogen protection, be warming up to 60 ~ 90 DEG C; Then add successively mol ratio be 1 ~ 1.4 phenylacrolein and mol ratio be the benzylideneacetone of 1, at temperature is 60 ~ 90 DEG C react 5 ~ 9h; Finally product is moved in vacuum rotary evaporator, at 90 DEG C, carry out underpressure distillation obtain this aldehyde ketone amine condenses inhibiter.
2. inhibiter preparation method according to claim 1, it is characterized in that: the application of aldehyde ketone amine condenses in acid solution inhibition that this preparation method obtains, it is the above-mentioned obtained aldehyde ketone amine condenses inhibiter of 0.8% of acid solution total amount by quality, joining massfraction is in the hydrochloric acid of 20%, is hung by A3 steel disc and immerses in above-mentioned hydrochloric acid soln, at temperature is 90 DEG C, soaks 4h, then take out, cleaning, dries, weighs; Through experiment detection display, the erosion rate of A3 steel disc is 3.14 ~ 4.75g/ (m
2h), corrosion inhibition rate is 99.91% ~ 99.94%; According to standard SY/T 5405-1996 first grade require regulation, at 90 DEG C 20% concentrated hydrochloric acid in corrosion speed be 3 ~ 5g/ (m
2h).Prove that this inhibiter has reached first grade required standard by experiment.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987822A (en) * | 2017-12-06 | 2018-05-04 | 唐山市金沙工贸有限公司 | High-temperature acidification corrosion inhibitor and preparation method thereof and application |
| CN110283581A (en) * | 2018-03-19 | 2019-09-27 | 中国石油天然气股份有限公司 | Acidification corrosion inhibitor suitable for 160 DEG C or more high temperature |
| CN110577829A (en) * | 2018-06-08 | 2019-12-17 | 中国石油天然气股份有限公司 | Cinnamaldehyde Schiff base acidizing corrosion inhibitor, preparation and use method |
| CN111748048A (en) * | 2020-08-03 | 2020-10-09 | 西南石油大学 | Preparation method of modified chitosan acidizing corrosion inhibitor |
-
2015
- 2015-07-09 CN CN201510397228.3A patent/CN104910028A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 刘俊等: "一种苄叉丙酮Mannich 碱缓蚀剂的合成及其缓蚀性能", 《材料保护》 * |
| 李建波等: "Mannich反应在酸化缓蚀剂合成中的应用", 《精细与专用化学品》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987822A (en) * | 2017-12-06 | 2018-05-04 | 唐山市金沙工贸有限公司 | High-temperature acidification corrosion inhibitor and preparation method thereof and application |
| CN110283581A (en) * | 2018-03-19 | 2019-09-27 | 中国石油天然气股份有限公司 | Acidification corrosion inhibitor suitable for 160 DEG C or more high temperature |
| CN110577829A (en) * | 2018-06-08 | 2019-12-17 | 中国石油天然气股份有限公司 | Cinnamaldehyde Schiff base acidizing corrosion inhibitor, preparation and use method |
| CN111748048A (en) * | 2020-08-03 | 2020-10-09 | 西南石油大学 | Preparation method of modified chitosan acidizing corrosion inhibitor |
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Application publication date: 20150916 |
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