CN103865506B - High-temperature acidizing corrosion inhibitor for oil-gas fields and preparation method thereof - Google Patents
High-temperature acidizing corrosion inhibitor for oil-gas fields and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/72—Eroding chemicals, e.g. acids
- C09K8/74—Eroding chemicals, e.g. acids combined with additives added for specific purposes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
- C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
- C02F5/12—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances containing nitrogen
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- C07D233/04—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D233/06—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
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- C07D233/04—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D233/06—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
- C07D233/08—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms with alkyl radicals, containing more than four carbon atoms, directly attached to ring carbon atoms
- C07D233/12—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms with alkyl radicals, containing more than four carbon atoms, directly attached to ring carbon atoms with substituted hydrocarbon radicals attached to ring nitrogen atoms
- C07D233/14—Radicals substituted by oxygen atoms
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- 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
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/14—Nitrogen-containing compounds
- C23F11/149—Heterocyclic compounds containing nitrogen as hetero atom
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/32—Anticorrosion additives
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Abstract
The invention relates to a method for preparing a high-temperature acidizing corrosion inhibitor for oil-gas fields. The method comprises the following steps: firstly a certain amount of alkynol, a formaldehyde solution and imidazoline are added into a reaction kettle with a mixer and a condensing device, and simultaneously the pH value is adjusted using hydrochloric acid; the condensing device is turned on, heating and mixing are started, a mannich base is obtained based on reflux reaction, and excessive formaldehyde and hydrogen chloride are removed by vacuum distillation; then a quaternization reagent is dripped into the mannich base, and the mixture is heated and maintained the temperature for continuous reaction to obtain mannich quaternary ammonium salt, wherein the mole ratio of alkynol, formaldyhyde and imidazoline is 1:1.0-1.5:1, the pH value of the reaction system is smaller than or equal to 2, the reaction temperature is 80-120 DEG C, and the reaction time is 3-10 hours; the quaternization reagent is chlorohydrocarbon, the dripping speed is 300-1000 kg/h per ton of production capacity, the reaction temperature of quatermization is 90-120 DEG C, and the reaction time is 3-7 hours.
Description
Technical field
The present invention relates to a kind of water treatment agent and preparation method thereof, particularly relate to a kind of oil gas field high-temperature acidification corrosion inhibitor
And preparation method thereof.
Background technology
Acidifying is one of effective measures that oil gas field increases augmented injection, but acid solution is to oil well metal equipment and oil-gas pipeline
Corroding more serious, in addition going deep into along with exploitation of oil-gas field, increasing high temperature well starts appearance, and this is to acidification corrosion inhibitor
Require more and more higher.In recent years, in Inhibitor For Oil Well System research field, done substantial amounts of research work both at home and abroad, achieved considerable
Progress, develops a series of acidification corrosion inhibitor new varieties.But the research to high-temperature acidification corrosion inhibitor is little, therefore studies performance
Superior high-temperature acidification corrosion inhibitor seems even more important.
The high-temperature acidification corrosion inhibitor used the earliest is arsenic salt, but owing to it has toxicity, can cause environmental pollution, by
Abandon.
Summary of the invention
It is an object of the invention to provide a kind of acid-soluble good, corrosion mitigating effect oil gas field notable, safety and environmental protection high temperature acidified
Corrosion inhibiter and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is:
The preparation method of a kind of oil gas field high-temperature acidification corrosion inhibitor, is characterized in that, operating procedure is: first, equipped with stirring
Mix and add a certain amount of alkynol, formalin and imidazoline in the reactor of condensing unit, regulate pH value with hydrochloric acid simultaneously；Beat
Driving condensing unit, open heated and stirred, back flow reaction obtains Mannich base, and the structural formula of Mannich base is
, decompression is distilled off excess formaldehyde and hydrogen chloride；Then, graceful generate
Buddhist nun wishes dropping quaternizing agent in alkali, heats, keeps temperature, sustained response, i.e. obtains thing Mannich base quaternary ammonium salt.
According to the preparation method of described a kind of oil gas field high-temperature acidification corrosion inhibitor, it is characterized in that, described alkynol, described first
Aldehyde is 1:1.0 ~ 1.5:1 with the mol ratio of described imidazoline.
According to the preparation method of described a kind of oil gas field high-temperature acidification corrosion inhibitor, it is characterized in that, described alkynol, described first
Aldehyde is≤2 with the pH value of the reaction system of described imidazoline.
According to the preparation method of described a kind of oil gas field high-temperature acidification corrosion inhibitor, it is characterized in that, described alkynol, described first
The reaction temperature of aldehyde and described imidazoline is 80 ~ 120 DEG C, the response time is 3 ~ 10h.
According to the preparation method of described a kind of oil gas field high-temperature acidification corrosion inhibitor, it is characterized in that, described quaternized examination
Agent is chlorohydrocarbon.
According to the preparation method of described a kind of oil gas field high-temperature acidification corrosion inhibitor, it is characterized in that, described quaternizing agent
Rate of addition be production capacity 300 ~ 1000kg/h per ton.
According to the preparation method of described a kind of oil gas field high-temperature acidification corrosion inhibitor, it is characterized in that, described quaternized anti-
To answer temperature be 90 ~ 120 DEG C, the response time is 3 ~ 7h.
A kind of oil gas field high-temperature acidification corrosion inhibitor prepared by said method, is characterized in that, structural formula is
。
According to described a kind of oil gas field high-temperature acidification corrosion inhibitor, it is characterized in that, in described structural formula, n is the integer of 1 ~ 5.
According to described a kind of oil gas field high-temperature acidification corrosion inhibitor, it is characterized in that, R in described structural formula1For H or C2~17's
Saturated or unsaturated aliphatic hydrocarbon, R2For C4~20Aliphatic hydrocarbon or aromatic hydrocarbon.
Mannich class corrosion inhibiter is the acidification corrosion inhibitor of the class excellent performance that developed recently gets up, and is widely used in stone
During oil, natural gas produce, it it is the study hotspot of current corrosion inhibiter.
The invention discloses a kind of Mannich base quarternary ammonium salt compound, this compound is passed through with imidazoline by alkynol, formaldehyde
Mannich reaction produces Mannich base, is subsequently adding quaternizing agent reaction and prepares Mannich base quaternary ammonium salt.Dashing forward of this compound
Going out feature is that acid-soluble good, corrosion mitigating effect is notable, and consumption is few, and temperature tolerance is high, is soluble in the acid solution of room temperature to 135 DEG C,
Do not have layering and precipitating phenomenon, and, this Mannich base quaternary ammonium salt toxicity is low, safety and environmental protection.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1
One has structureThe synthetic method of Mannich base quaternary ammonium salt, preparation
Step is:
(1) in the reactor equipped with stirring and condensing unit, propilolic alcohol, formaldehyde and imidazoline, propilolic alcohol: first are added
Aldehyde: the mol ratio of imidazoline is 1:1.2:1, simultaneously with hydrochloric acid regulation pH value to 1.5.Open condensing unit, open stirring, heating
Obtaining Mannich base to 100 DEG C of back flow reaction 5h, decompression is distilled off excess formaldehyde and hydrogen chloride.
(2) with the speed dropping chlorinated dodecane of 800kg/h in the Mannich base generated, it is heated to 100 DEG C and keeps temperature
Degree, sustained response 5h, i.e. obtain the Mannich base quaternary ammonium salt of said structure.
Embodiment 2
One has structureThe synthetic method of Mannich base quaternary ammonium salt,
Preparation process is:
(1) in the reactor equipped with stirring and condensing unit, propilolic alcohol, formaldehyde and imidazoline, propilolic alcohol: first are added
Aldehyde: the mol ratio of imidazoline is 1:1.3:1, simultaneously with hydrochloric acid regulation pH value to 1.5.Open condensing unit, open stirring, heating
Obtaining Mannich base to 100 DEG C of back flow reaction 5h, decompression is distilled off excess formaldehyde and hydrogen chloride.
(2) with the speed dropping benzyl chloride of 500kg/h in the Mannich base generated, it is heated to 100 DEG C and keeps temperature, hold
Continuous reaction 4h, i.e. obtains the Mannich base quaternary ammonium salt of said structure.
Embodiment 3
One has structureThe synthetic method of Mannich base quaternary ammonium salt, preparation
Step is:
(1) in the reactor equipped with stirring and condensing unit, propilolic alcohol, formaldehyde and imidazoline, propilolic alcohol: first are added
Aldehyde: the mol ratio of imidazoline is 1:1.3:1, simultaneously with hydrochloric acid regulation pH value to 2.0.Open condensing unit, open stirring, heating
Obtaining Mannich base to 90 DEG C of back flow reaction 7h, decompression is distilled off excess formaldehyde and hydrogen chloride.
(2) with the speed dropping benzyl chloride of 500kg/h in the Mannich base generated, it is heated to 100 DEG C and keeps temperature, hold
Continuous reaction 4h, i.e. obtains the Mannich base quaternary ammonium salt of said structure.
Embodiment 4
One has structureThe synthetic method of Mannich base quaternary ammonium salt, preparation
Step is:
(1) in the reactor equipped with stirring and condensing unit, propilolic alcohol, formaldehyde and imidazoline, propilolic alcohol: first are added
Aldehyde: the mol ratio of imidazoline is 1:1.5:1, simultaneously with hydrochloric acid regulation pH value to 1.0.Open condensing unit, open stirring, heating
Obtaining Mannich base to 110 DEG C of back flow reaction 8h, decompression is distilled off excess formaldehyde and hydrogen chloride.
(2) with the speed dropping chloro heptane of 500kg/h in the Mannich base generated, it is heated to 100 DEG C and keeps temperature,
Sustained response 6h, i.e. obtains the Mannich base quaternary ammonium salt of said structure.
Embodiment 5
One has structureThe synthetic method of Mannich base quaternary ammonium salt,
Preparation process is:
(1) in the reactor equipped with stirring and condensing unit, propilolic alcohol, formaldehyde and imidazoline, propilolic alcohol: first are added
Aldehyde: the mol ratio of imidazoline is 1:1.2:1, simultaneously with hydrochloric acid regulation pH value to 1.0.Open condensing unit, open stirring, heating
Obtaining Mannich base to 110 DEG C of back flow reaction 6h, decompression is distilled off excess formaldehyde and hydrogen chloride.
(2) with the speed dropping chloro heptane of 500kg/h in the Mannich base generated, it is heated to 100 DEG C and keeps temperature,
Sustained response 6h, i.e. obtains the Mannich base quaternary ammonium salt of said structure.
Embodiment described above is only to be described the preferred embodiment of the present invention, the not structure to the present invention
Thinking and scope is defined, on the premise of without departing from design concept of the present invention, in this area, ordinary skill technical staff is to this
The various modification made of technical scheme of invention and improvement, all should fall into protection scope of the present invention, and the present invention is claimed
Technology contents, all records in detail in the claims.
Claims (7)
1. a preparation method for oil gas field high-temperature acidification corrosion inhibitor, is characterized in that, operating procedure is: first, equipped with stirring
With the reactor of condensing unit adds a certain amount of alkynol, formalin and imidazoline, use salt acid for adjusting pH value simultaneously；Beat
Driving condensing unit, open heated and stirred, back flow reaction obtains Mannich base, and the structural formula of Mannich base is,
In structural formula, n is the integer of 1 ~ 5, R1For H or C2~17Saturated or unsaturated aliphatic hydrocarbyl moiety；Decompression is distilled off excess first
Aldehyde and hydrogen chloride；Then, the Mannich base generated drips quaternizing agent, heats, keep temperature, sustained response, to obtain final product
To Mannich base quaternary ammonium salt.
The preparation method of a kind of oil gas field high-temperature acidification corrosion inhibitor the most according to claim 1, is characterized in that, alkynol, first
Aldehyde is 1:1.0 ~ 1.5:1 with the mol ratio of imidazoline.
The preparation method of a kind of oil gas field high-temperature acidification corrosion inhibitor the most according to claim 1, is characterized in that, alkynol, first
PH value≤2 of the reaction system of aldehyde and imidazoline.
The preparation method of a kind of oil gas field high-temperature acidification corrosion inhibitor the most according to claim 1, is characterized in that, alkynol, first
The reaction temperature of aldehyde and imidazoline is 80 ~ 120 DEG C, the response time is 3 ~ 10h.
The preparation method of a kind of oil gas field high-temperature acidification corrosion inhibitor the most according to claim 1, is characterized in that, described season
Ammonium reagent is chlorohydrocarbon.
The preparation method of a kind of oil gas field high-temperature acidification corrosion inhibitor the most according to claim 1, is characterized in that, quaternized
Reaction temperature is 90 ~ 120 DEG C, the response time is 3 ~ 7h.
7. the oil gas field high-temperature acidification corrosion inhibitor prepared by method according to any one of claim 1 to 6, is characterized in that,
Structural formula is
In structural formula, n is the integer of 1 ~ 5, R1For H or C2~17Saturated or unsaturated aliphatic hydrocarbyl moiety, R2For benzyl or C4~20Fat
Alkyl.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2532990A (en) | 2014-12-05 | 2016-06-08 | Schlumberger Holdings | Corrosion inhibition |
| GB2543498A (en) | 2015-10-19 | 2017-04-26 | Schlumberger Holdings | Corrosion inhibition |
| CN106478510B (en) * | 2016-09-14 | 2018-01-30 | 武汉楚博士科技有限公司 | Alkynol base imidazolinium compounds, the corrosion inhibiter for carbon dioxide drive and preparation |
| CN108239772B (en) * | 2016-12-27 | 2020-03-10 | 中国石油天然气股份有限公司 | Corrosion inhibitor for oil-water interface of ground gathering and transportation system and preparation method thereof |
| CN107573914A (en) * | 2017-08-29 | 2018-01-12 | 中国石油集团渤海钻探工程有限公司 | A kind of compound acidification corrosion inhibitor based on Mannich base and BAA |
| CN111499527B (en) * | 2020-06-08 | 2023-04-07 | 中国石油大学(华东) | Preparation method and application of high-temperature-resistant acidizing corrosion inhibitor of crosslinked acid system |
| CN113106457A (en) * | 2021-04-08 | 2021-07-13 | 四川瑞冬科技有限公司 | Corrosion inhibitor and preparation method thereof |
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| CN100591803C (en) * | 2006-09-04 | 2010-02-24 | 中国石油集团川庆钻探工程有限公司 | Corrosion inhibitor resistant to H2S and CO2 |
| CN101654303B (en) * | 2008-08-18 | 2011-05-04 | 天津大港油田科远石油工程有限责任公司 | Corrosion inhibitor suitable for complex wastewater of oilfield and preparation method thereof |
| CN101892042B (en) * | 2010-06-30 | 2013-03-20 | 中国海洋石油总公司 | High temperature acidizing corrosion inhibitor and preparation method thereof |
| CN102049213B (en) * | 2010-11-12 | 2013-06-19 | 西华师范大学 | Propargyl alcohol type quaternary ammonium salt surfactant and preparation method thereof |
| CN102953067B (en) * | 2011-08-19 | 2014-11-26 | 中国石油天然气股份有限公司 | Decalcification Mannich base corrosion inhibitor, and preparation and application thereof |
| CN103014715B (en) * | 2012-08-09 | 2014-09-10 | 江苏科技大学 | Corrosion inhibitor composition for preventing hydrogen sulfide corrosion |
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