CN107523287A - A kind of combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt - Google Patents
A kind of combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt Download PDFInfo
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- CN107523287A CN107523287A CN201710756719.1A CN201710756719A CN107523287A CN 107523287 A CN107523287 A CN 107523287A CN 201710756719 A CN201710756719 A CN 201710756719A CN 107523287 A CN107523287 A CN 107523287A
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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
- 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
- C09K8/54—Compositions for in situ inhibition of corrosion in boreholes or wells
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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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/32—Anticorrosion additives
Abstract
The invention discloses a kind of combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt, including 20~30 parts of corrosion inhibiter hosts, 2.0~2.5 parts of synergist, 0.2~1.0 part of dispersant, 0.5~1.0 part of propilolic alcohol, 0.2~1 part of emulsifying agent, 2.5~6.0 parts of triethanolamines, 0.8~1.0 part of surfactant and 60~70 parts of solvents in parts by weight；Corrosion inhibiter host is using pyridine quaternary ammonium salt made of 3 picolines and benzyl chloride reaction；Synergist is the mixture of KI, antimony oxide and antimony trichloride, and three's weight ratio is 2~3:1~2:1~2；The combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt meets the acidification of oil field construction requirement under the conditions of 120~160 DEG C, there is provided that a kind of property is stable, corrosion inhibition is good, is easy to site operation and the corrosion inhibitor formula of cost advantage, the corrosion inhibiter has good and good with conventional imidazoline inhibitor, other kinds of quaternary ammonium salt corrosion inhibitor compatibility with the conventional acidizing additive compatibility in scene, can be used in mixed way, easy for construction and high safety, it is pollution-free, convenience in transport storage is low with cost the features such as.
Description
Technical field
It is more particularly to a kind of based on the compound of pyridines quaternary ammonium salt the present invention relates to acidification of oil field construction operation technical field
High-temperature acidification corrosion inhibitor.
Background technology
In acidification of oil gas well, particularly in high temperature deep well and ultradeep well carry out concentrated hydrochloric acid or a large amount of acid acidifyings, primarily
Task be to solve etching problem of the high temperature acidified liquid to oil well casing equipment.In acid cleaning process, especially inorganic acid is matched somebody with somebody
The pickle of system, it causes a certain degree of corrosion and destruction to hardware and material.
With the development of drilling technology and the progress of oil recovery technique, a large amount of deep-wells, ultradeep well input exploitation, measure amount is acidified
Increase year by year, higher requirement it is also proposed with the performance of corrosion inhibiter to acidifying.Well of the well temperature more than 120 DEG C, acidification corrosion inhibitor
Performance is greatly reduced, although part well can realize the purpose of inhibition by way of the well-flushing cooling before acidifying, if
Occur abnormal midway termination of pumping or the well without well-flushing condition in acidization, then can not realize.In addition, after metal and acid reaction
Caused hydrogen can cause hydrogen embrittlement to corrode hardware, and can also take substantial amounts of sour gas out of and form acid mist, in high temperature
Under the conditions of meeting further such that underground operation tool and down-hole string working condition deteriorate, it is therefore necessary to metal under hot environment
Corrosion take targetedly inhibition measure.High-temperature acidification corrosion inhibitor be mainly used in preventing during high-temperature oil well acidizing treatment hydrochloric acid or
Corrosion of the mud acid solution to hardware or down-hole string, to ensure the implementation of oil well acidation fracturing technology and volume increase, stable yields skill
The realization of art measure.When the oil field high temperature deep well having in the past is using concentrated hydrochloric acid acidifying oil well, because not preferable corrosion inhibiter is prevented
Corruption, the accidents such as down-hole oil tube dropout often occur.Therefore, in HTHP oil well acidation work progress, exactly it is close in acid solution
Add high-temperature acidification corrosion inhibitor and suppress corrosion of the acid solution to down-hole string.
The content of the invention
It is an object of the invention to provide a kind of acidification of oil field construction of temperature suitable for Oil/gas Well at 120~160 DEG C
Combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt.
Therefore, technical solution of the present invention is as follows：
A kind of combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt, including 20~30 parts of inhibitions in parts by weight
Agent host, 2.0~2.5 parts of synergist, 0.2~1.0 part of dispersant, 0.5~1.0 part of propilolic alcohol, 0.2~1 part of emulsifying agent, 2.5
~6.0 parts of triethanolamines, 0.8~1.0 part of surfactant and 60~70 parts of solvents.
Wherein, the corrosion inhibiter host is that it is tied using pyridine quaternary ammonium salt made of 3- picolines and benzyl chloride reaction
Structure formula is as shown in following formula I：
The quaternized pyridinium salt production process is simple, and its specific preparation process is：It is 1 by mol ratio:3 3- picolines with
Benzyl chloride is added in reaction bulb, is added 0.8~1.2 times of reactant gross mass aqueous solvent, is stirred to reactant and be completely dissolved；Drop
Add hydrochloric acid conditioning solution pH to 7~8, and be warming up to 90~100 DEG C, 5~6h of reaction time, obtain crude product；Petroleum ether extraction is thick
Product, and the mixed solution of the product after extraction and petroleum ether is dried in vacuo to remove petroleum ether, that is, obtain pyridine quaternary ammonium salt
Product.
Specific chemical reaction reaction equation is as follows：
Specifically, the synergist is the mixture of KI, antimony oxide and antimony trichloride, and three's weight ratio is 2
~3:1~2:1~2.
It is preferred that the dispersant is OP-10, i.e. polyoxethylene octylphenyl phenol ether -10, it is a kind of colourless or clear yellow viscous
Liquid.
It is preferred that the surfactant is sodium n-alkylbenzenesulfonate, referred to as LAS, molecular formula C18H30O3S。
It is preferred that the emulsifying agent is paregal O, i.e. alkyl polyoxyethylene ether；Actually preparing combined high temperature acidifying inhibition
During agent, can optionally any model paregal O as emulsifying agent.
It is preferred that the solvent is DMF (DMF), the N of 2~10 parts by weight, N- bis- of 2~10 parts by weight
The mixture of the methanol of methylbenzene (DMA) and 41~66 parts by weight.
Have by the composite corrosion inhibitor formed after being compounded in proportion with synergist, dispersant, surfactant and solvent
More stable property, preferable corrosion inhibition is shown in the hydrochloric acid and mud acid under 120~160 DEG C of environment.It is used for oil
Dosage when field acidizing treatment additive uses is 2.0~4.0wt.%.
The beneficial effect of the combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt is：
(1) the combined high temperature acidification corrosion inhibitor is in 0~20wt.%HCl and mud acid system (12wt.%HCl and 3wt.%
HF in), N80 steel discs, inhibition speed reaches SY/T 5405-1996 first class index under 120~160 DEG C of temperature conditionss, is fully able to
Suitable for operations such as acidification of oil gas well, acid fracturing volume increase；
(2) the combined high temperature acidification corrosion inhibitor its corrosion inhibition under the conditions of 160 DEG C maintains more than 3 days, or it is longer when
Interior can stablize play its corrosion inhibition, improve the acidizing treatment quality under the conditions of 160 DEG C；
(3) through not putrid and deteriorated in long-time storage and transportation process, centralized system is standby to answer the combined high temperature acidification corrosion inhibitor
The acidizing treatment measures to reform that corrosion inhibiter is easy to distribution to multiple wells is closed, onsite application is all easier, only need to be required
2.0~4.0wt.% is added in acid fluid system and can reach good corrosion mitigating effect；
(4) the combined high temperature acidification corrosion inhibitor has preferable compatibility with conventional acidification of oil field system.This is compound slow
Losing agent can be with conventional acid system and acidizing additive (such as clay stabilizer, ferrous stability, demulsification cleanup agent, precipitation
Inhibitor etc.) preferable compatibility is respectively provided with, precipitation will not be produced.It is easy to be compounded with different acid systems, uses model
Enclose wide；
(5) the combined high temperature acidification corrosion inhibitor property is stable, and chance naked light is non-ignitable, and working security is high；
(6) raw material of the combined high temperature acidification corrosion inhibitor easily obtains, and host preparation method is simple, is advantageous to scale metaplasia
Production.
Embodiment
With reference to specific embodiment, the present invention is described further, but following embodiments absolutely not to the present invention have appoint
What is limited.
The dosage of each component is parts by weight in example 1 below~5.
Embodiment 1
A kind of combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt, including 20 parts of corrosion inhibiter hosts, 1.0 parts of iodate
Potassium, 0.5 part of antimony oxide, 0.5 part of antimony trichloride, 0.5 paregal O -15,0.5 part of propilolic alcohol, 1.0 parts of OP-10,6.0 part three
Monoethanolamine, 1.0 parts of LAS, 7.0 parts of DMF, 7.0 parts of DMA, 55 parts of methanol.In use, puddled after said components are weighed uniformly i.e.
Job site can be sent into use or store stand-by.
Embodiment 2
A kind of combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt, including 22 parts of corrosion inhibiter hosts, 1.5 parts of iodate
Potassium, 0.5 part of antimony oxide, 0.5 part of antimony trichloride, 0.2 part of paregal O -20,0.8 part of propilolic alcohol, 0.2 part of OP-10,2.5 parts
Triethanolamine, 0.8 part of LAS, 3.0 parts of DMF, 3.0 parts of DMA, 64 parts of methanol.In use, puddled after said components are weighed uniformly
Job site can be sent into use or store stand-by.
Embodiment 3
A kind of combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt, including 25 parts of corrosion inhibiter hosts, 1.2 parts of iodate
Potassium, 0.6 part of antimony oxide, 0.7 part of antimony trichloride, 0.5 part of peregal O-25,1.0 parts of propilolic alcohols, 0.5 part of OP-10,3.5 parts
Triethanolamine, 1.0 parts of LAS, 2.0 parts of DMF, 5.0 parts of DMA, 59 parts of methanol.In use, puddled after said components are weighed uniformly
Job site can be sent into use or store stand-by.
Embodiment 4
A kind of combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt, including 25 parts of corrosion inhibiter hosts, 1.0 parts of iodate
Potassium, 0.5 part of antimony oxide, 1.0 parts of antimony trichlorides, 0.5 part of peregal O-25,1.0 parts of propilolic alcohols, 0.3 part of OP-10,2.7 parts
Triethanolamine, 1.0 parts of LAS, 3.0 parts of DMF, 4.0 parts of DMA, 60 parts of methanol.In use, puddled after said components are weighed uniformly
Job site can be sent into use or store stand-by.
Embodiment 5
A kind of combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt, including 27 parts of corrosion inhibiter hosts, 1.5 parts of iodate
Potassium, 0.5 part of antimony oxide, 0.5 part of antimony trichloride, 0.5 part of paregal O -30,0.5 part of propilolic alcohol, 0.5 part of OP-10,4.0 parts
Triethanolamine, 1.0 parts of LAS, 4.0 parts of DMF, 4.0 parts of DMA, 56 parts of methanol.In use, puddled after said components are weighed uniformly
Job site can be sent into use or store stand-by.
In above-described embodiment 1~5 in addition to corrosion inhibiter host, remaining each component and prepare corrosion inhibiter host raw material it is equal
Buy from commercially available prod.
The specific preparation method of corrosion inhibiter host is：0.2mol 3- picolines and 0.6mol benzyl chlorides are added three mouthfuls
In flask, 100g aqueous solvents are then added, stirs to 3- picolines and benzyl chloride and is dissolved completely in water；Dripped into reaction solution
Add 37.5wt.% hydrochloric acid to adjust pH=7.5, and be warming up to 90 DEG C, reaction 6h, obtain crude product；With petroleum ether to crude product
Extracted, then extraction product is put into vacuum drying chamber and dried, petroleum ether is removed, obtains pyridine quaternary ammonium salt end-product.
Performance test：
The combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt prepared to above-described embodiment 1~5 is respectively from inhibition
Performance, dissolution dispersity energy, core permeability infringement experiment etc. are tested.
(1) corrosion inhibition is tested：
Corrosion mitigating effect of the temperature higher than more than 90 DEG C is evaluated, with reference to People's Republic of China's oil and gas industry standard
SY/T 5405-1996《Corrosion inhibiter method for testing performance and evaluation index are used in acidifying》In HTHP Dynamic Corrosion speed survey
The method of determining is evaluated.The sample prepared is poured into high temperature and high pressure kettle, then the test piece handled well is put into kettle, temperature
When reaching assigned temperature, start timing, reaction is taken out test piece after 4 hours and handled, and calculates average corrosion rate.Test result
It is as shown in table 1 below.
Table 1：
From upper table 1 as can be seen that under the conditions of 120 DEG C, in 15wt.% HCl, 20wt.% HCl and 12wt.%
In HCl+3.0wt.%HF, 2% dosage can reach SY/T 5405-1996 one-level performance indications；Under the conditions of 140 DEG C,
In 15wt.%HCl, 20wt.%HCl and 12wt.%HCl+3.0wt.%HF, 2.5wt.% dosage can reach SY/T
5405-1996 one-level performance indications；Under the conditions of 160 DEG C, in 15wt.%HCl, 20wt.%HCl and 12wt.%HCl+
In 3.0wt.%HF, 4wt.% dosage can reach SY/T 5405-1996 one-level performance indications.It can be seen that the compound acidifying being somebody's turn to do
Inhibition speed reaches the production of petroleum industry standard SY/T 5405-1996 corrosion inhibiter one-level under the conditions of below 120~160 DEG C of corrosion inhibiter
The index request of product.
Further choose respectively compound acidification corrosion inhibitor prepared by embodiment 1~5 tested at 160 DEG C of test temperature its
The corrosion rate after 72h is reacted in different proportion acid solution, test result is referring to table 2 below.
Table 2：
From table 2 it can be seen that under the conditions of 160 DEG C, in 15wt.%HCl, 20wt.%HCl, 12wt.%HCl+3wt.%
Though the corrosion rate of steel is increased slightly after 72h but be able to can still reached one specified in SY/T 5405-1996 in HF
Level performance indications.It can be seen that the corrosion inhibiter its corrosion inhibition under the conditions of 160 DEG C maintains more than 3 days, or can in the longer time
It is stable to play its corrosion inhibition, the acidizing treatment quality being effectively improved under the conditions of 160 DEG C.
(2) dissolution dispersity can be tested：
According to SY/T 5405-1996《Corrosion inhibiter method for testing performance and evaluation index are used in acidifying》In corrosion inhibiter dissolving
Dispersed assay method and evaluation index, by the way that well mixed is contained into a certain proportion of combined high temperature acidification corrosion inhibitor
Acid solution bottle be put into the water-bath of constant temperature, the situation of change for observing acid solution outward appearance evaluates the dissolution dispersity of corrosion inhibiter.
Test result is as shown in table 3 below.
Table 3：
| Sequence number | Time, h | Dissolve deployment conditions | Index |
| Embodiment one | 36 | Acid solution transparent clear, aneroid/stratified liquid, aneroid/solid phase separation | One-level |
| Embodiment two | 36 | Acid solution transparent clear, aneroid/stratified liquid, aneroid/solid phase separation | One-level |
| Embodiment three | 36 | Acid solution transparent clear, aneroid/stratified liquid, aneroid/solid phase separation | One-level |
| Example IV | 36 | Acid solution transparent clear, aneroid/stratified liquid, aneroid/solid phase separation | One-level |
| Embodiment five | 36 | Acid solution transparent clear, aneroid/stratified liquid, aneroid/solid phase separation | One-level |
Can be seen that the combined high temperature acidification corrosion inhibitor from the test result of upper table 3 has preferable compatibility, with commonly using
Occurred after acid solution mixing in 36 hours without the scene such as precipitation, layering.
(3) corrosion inhibiter is damaged to core permeability and tested：
According to SY/T 5405-1996《Corrosion inhibiter method for testing performance and evaluation index are used in acidifying》In corrosion inhibiter rock core
Permeability impairment is tested, and the combined high temperature acidification corrosion inhibitor aqueous solution of 2.5% concentration is squeezed into natural core, flowed with rock core
The permeability of the forward and backward natural core of the corrosion inhibiter aqueous solution, the degree that measure corrosion inhibiter damages to core permeability are squeezed into instrument measurement.
Corrosion inhibiter is calculated by formula (1) the loss ratio of core permeability：
In formula：μiThe loss ratio of-core permeability, %；
K0, Ki- corrosion inhibiter the aqueous solution injects forward and backward kerosene and surveys permeability, and 10-3μm2；
I=1,2,3,4,5.
Test result is as shown in table 4 below.Wherein, rock core 1 uses product prepared by corrosion inhibiter embodiment 1, rock in table 4
The heart 2 uses product prepared by corrosion inhibiter embodiment 2, by that analogy.
Table 4：
| Rock core | K0, 10‐3μm2 | Ki, 10‐3μm2 | Permeability damage rate, % |
| 1 | 22.12 | 20.16 | 8.86 |
| 2 | 20.73 | 19.14 | 7.67 |
| 3 | 25.73 | 23.72 | 7.81 |
| 4 | 19.71 | 18.12 | 8.07 |
| 5 | 21.48 | 19.92 | 7.26 |
As can be seen from Table 4, the permeability damage rate in above-mentioned five kinds of acid fluid systems has preferable below 9%
Reservoir protection performance, disclosure satisfy that in actual production to the needs of reservoir protection.
In addition, the combined high temperature acidification corrosion inhibitor is in actual use, added with conventional acid system and acidifying
Agent (such as clay stabilizer, ferrous stability, demulsification cleanup agent, precipitating inhibitor) is respectively provided with preferable compatibility, will not
Produce precipitation.It is easy to be compounded with different acid systems, use range is wide.
Claims (6)
1. a kind of combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt, it is characterised in that including 20 in parts by weight
~30 parts of corrosion inhibiter hosts, 2.0~2.5 parts of synergist, 0.2~1.0 part of dispersant, 0.5~1.0 part of propilolic alcohol, 0.2~1 part
Emulsifying agent, 2.5~6.0 parts of triethanolamines, 0.8~1.0 part of surfactant and 60~70 parts of solvents；Wherein,
The corrosion inhibiter host is using pyridine quaternary ammonium salt, its structural formula such as following formula made of 3- picolines and benzyl chloride reaction
Shown in I：
The synergist is the mixture of KI, antimony oxide and antimony trichloride, and three's weight ratio is 2~3:1~2:1~2.
2. the combined high temperature acidification corrosion inhibitor according to claim 1 based on pyridines quaternary ammonium salt, it is characterised in that described
The preparation method of corrosion inhibiter host is：It is 1 by mol ratio:3 3- picolines are added in reaction bulb with benzyl chloride, add 0.8
~1.2 times of reactant gross mass aqueous solvents, stir to reactant and are completely dissolved；Hydrochloric acid conditioning solution pH is added dropwise to 7~8, and
90~100 DEG C, 5~6h of reaction time are warming up to, obtains crude product；Petroleum ether extraction crude product, and by the product and stone after extraction
The mixed solution of oily ether is dried in vacuo to remove petroleum ether, that is, obtains pyridine quaternary ammonium salt product.
3. the combined high temperature acidification corrosion inhibitor according to claim 1 based on pyridines quaternary ammonium salt, it is characterised in that described
Dispersant is OP-10.
4. the combined high temperature acidification corrosion inhibitor according to claim 1 based on pyridines quaternary ammonium salt, it is characterised in that described
Surfactant is sodium n-alkylbenzenesulfonate.
5. the combined high temperature acidification corrosion inhibitor according to claim 1 based on pyridines quaternary ammonium salt, it is characterised in that described
Solvent is by the N of the N,N-dimethylformamide of 2~10 parts by weight, 2~10 parts by weight, accelerine and 41~66 weight
The mixed solvent that the methanol of part mixes.
6. the combined high temperature acidification corrosion inhibitor according to claim 1 based on pyridines quaternary ammonium salt, it is characterised in that described
Emulsifying agent is paregal O.
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| CN110484922A (en) * | 2018-05-15 | 2019-11-22 | 中国石油天然气股份有限公司 | A kind of gas-liquid two-phase carbon dioxide corrosion inhibitor and preparation method thereof |
| CN108796507A (en) * | 2018-07-06 | 2018-11-13 | 佛山陵朝新材料有限公司 | A kind of compound acidification corrosion inhibitor |
| CN109294549A (en) * | 2018-08-30 | 2019-02-01 | 赵晴晴 | A kind of high temperature oil field acidification corrosion inhibitor and preparation method |
| CN109251742A (en) * | 2018-09-29 | 2019-01-22 | 中国石油天然气集团有限公司 | A kind of visco-elastic surfactant acid corrosion inhibiter and preparation method thereof |
| CN109251742B (en) * | 2018-09-29 | 2022-03-01 | 中国石油天然气集团有限公司 | Corrosion inhibitor for clean diverting acid and preparation method thereof |
| CN109776402A (en) * | 2019-01-30 | 2019-05-21 | 深圳市兆新能源股份有限公司 | Isopropylamine yl pyridines quaternary ammonium salt and preparation method thereof and aqueous cleaning aerosol |
| CN113278409A (en) * | 2021-06-22 | 2021-08-20 | 西南石油大学 | High-temperature acidizing corrosion inhibitor |
| CN113278409B (en) * | 2021-06-22 | 2022-04-29 | 西南石油大学 | High-temperature acidizing corrosion inhibitor |
| CN114574183A (en) * | 2022-02-15 | 2022-06-03 | 陕西化工研究院有限公司 | CO (carbon monoxide)2Imidazoline-pyridine composite corrosion inhibitor for oil displacement |
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