CN106367057A - Corrosion inhibitor used for acidizing and resisting to high temperature of 140-160 DEG C and preparation method for inhibitor - Google Patents
Corrosion inhibitor used for acidizing and resisting to high temperature of 140-160 DEG C and preparation method for inhibitor Download PDFInfo
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- CN106367057A CN106367057A CN201610742047.4A CN201610742047A CN106367057A CN 106367057 A CN106367057 A CN 106367057A CN 201610742047 A CN201610742047 A CN 201610742047A CN 106367057 A CN106367057 A CN 106367057A
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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
- C09K8/725—Compositions containing polymers
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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
- 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
- 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
- C23F11/04—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in markedly acid liquids
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Abstract
The invention discloses a corrosion inhibitor used for acidizing and resisting to high temperature of 140-160 DEG C. The corrosion inhibitor is prepared from, by weight, 20-30% of composite alkyl pyridine quaternary ammonium salt, 4-8% of fatty alcohol-polyoxyethylene ether, 4-8% of organic aldehyde, 2-4% of alkynol, 25-30% of organic acid, 5-10% of organic alcohol and water. The corrosion inhibitor has good dispersibility, good compatibility and less coke formation in an acid liquor, and is suitable for acid stimulation operating construction in a deep well; under the condition that the use amount of the corrosion inhibitor is only 2%, the corrosion rate is less than or equal to 20 g/(m<2>.h) which is much better than the standard of industry first-grade products, and the corrosion inhibition effect is very good. Moreover, raw materials used in the corrosion inhibitor are easy to obtain, reaction conditions are mild and production process is simple; obviously, the corrosion of the acid liquid to the device and pipe columns is reduced with the largest limit, and thus the successful construction of the high-temperature acidizing construction is ensured.
Description
Technical field
The present invention relates to inhibiter technology field, particularly to resistance to 140 DEG C～160 DEG C high temperature acidified use corrosion inhibiter of one kind and
Its preparation method.
Background technology
It is often necessary to recovery ratio is improved by acidifying during oil gas well mining.But during acidizing treatment, acid
Liquid not only can damage ground installation and down-hole string to corrosion of metal, and a large amount of iron ions corroding are in certain condition
Under can form ferric hydroxide precipitate, affect acidizing effect, result even in the sudden break accident of downhole tubular goods.Acidifying working solution
The middle corrosion inhibiter adding coupling can reduce acid solution to the corrosion of equipment and tubing string to greatest extent it is ensured that acidizing treatment smoothly enters
OK.
Enter middle and late stage with oil field development, oil-gas mining difficulty is gradually increased, and each oil field is progressively to deep-well, ultradeep well
Exploitation is expanded, so, the Acidizing Technology service difficulty in domestic and international oil field is increasing, and the temperature needed for corrosion inhibiter is also increasingly
High.The requirement to corrosion inhibiter for the high-temperature stratum acidifying is higher, but the domestic at present acidifying being applied to 140 DEG C～160 DEG C of high temperature
Corrosion inhibiter kind is few, expensive, performance less stable, compatibility are poor, dissolution dispersity is bad etc..
Content of the invention
It is an object of the invention to provide a kind of compatibility is good, good dispersion, cheap, and can drop to greatest extent
Low acid solution is high temperature acidified to resistance to 140 DEG C～160 DEG C of the corrosion of equipment and tubing string to use corrosion inhibiter.
Another object of the present invention makes a kind of system preparing above-mentioned resistance to 140 DEG C～160 DEG C high temperature acidified use corrosion inhibiter of offer
Preparation Method.
For this reason, technical solution of the present invention is as follows:
A kind of resistance to 140 DEG C～160 DEG C high temperature acidified use corrosion inhibiter, including the component of following mass fraction:
Preferably, described compound alkyl pyridine quaternary ammonium salt passes through: 2,3,5- trimethylpyridines, 2,4- lutidines and 1- chlorine
Methyl naphthalene presses the amount of material ratio for 1:1:(3.0～3.5) occur quaterisation to generate；Or 2,4,6- trimethylpyridine, 2,5-
Lutidines and 2- bromomethyl naphthalene press the amount of material ratio for 1:1:(3.0～3.5) occur quaterisation to generate；Or 2,6- bis-
Picoline, 3- picoline and benzyl chloride press the amount of material ratio for 1:1:(3.0～3.5) occur quaterisation to generate.
Preferably, described fatty alcohol-polyoxyethylene ether is aeo-9, aeo-15 or aeo-20.
Wherein, fatty alcohol-polyoxyethylene ether, is also called aeo, and its structural formula is: r-o- (ch2ch2o)nh；Wherein, r=c12
～c18, n=9～20；Specifically:
Aeo-9 is it may be assumed that r-o- (ch2ch2o)9H, r=c12～c18；
Aeo-15 is it may be assumed that r-o- (ch2ch2o)15H, r=c12～c18；
Aeo-20 is it may be assumed that r-o- (ch2ch2o)20H, r=c12～c18；
Preferably, described organic aldehyde is formaldehyde, paraformaldehyde, acetaldehyde or cinnamic aldehyde；It is further preferred that described organic aldehyde be formaldehyde or
Cinnamic aldehyde.
Preferably, described alkynol propilolic alcohol, methyl butynol, methylparafynol, tertiary alkynol or dimethylated hexynol；More excellent
Choosing, described alkynol is propilolic alcohol or tertiary alkynol.
Preferably, described organic acid is formic acid or acetic acid.
Preferably, described Organic Alcohol is ethanol, isobutanol or ethylene glycol；It is further preferred that described Organic Alcohol is ethylene glycol.
A kind of preparation method preparing high temperature resistant acidifying corrosion inhibiter, comprises the steps:
S1, the synthesis of compound pyridine quaternary ammonium salt: pyridines monomer and Halogen group elements monomer are pressed the amount of material ratio for 2:
(2.0～2.5) ratio is completely dissolved in ethanol-water solution (vWater:vAlcohol=1:1) in, after 80～85 DEG C of isothermal reaction 3～3.5h,
Add the Halogen group elements monomer of the amount half being equivalent to pyridines monomeric substance, warming-in-water, to 94～99 DEG C, continues to stir
Mix reaction 2～2.5h, be slowly cooled to room temperature, obtain compound alkyl pyridine quaternary ammonium salt；
S2, the synthesis of corrosion inhibiter: fatty alcohol-polyoxyethylene ether is added to organic acid, stirs to making it be completely dissolved,
Form homogeneous mixing liquid i；Then sequentially add water, Organic Alcohol, alkynol, organic aldehyde in mixing liquid i, stir to make its mix
Close and uniformly obtain mixing liquid ii；The compound alkyl pyridine quaternary ammonium preparing through step s1 is added in the most backward mixing liquid ii
Salt, continues stirring 0.5～1h so as to uniform mix, that is, obtains high temperature resistant acidification corrosion inhibitor.
Preferably, the preparation method of this high temperature resistant acidifying corrosion inhibiter, including following concrete steps:
S1, the synthesis of compound pyridine quaternary ammonium salt: by 2,3,5- trimethylpyridine, 2,4- lutidines and 1- chloromethyl
Naphthalene, or 2，4，6-trimethylpyridine, 2,5- lutidines and 2- bromomethyl naphthalene, or 2,6- lutidines, 3- picoline
With benzyl chloride in material amount than for 2:(2.0～2.5) ratio is completely dissolved in ethanol-water solution (vWater:vAlcohol=1:1) in, 80
After～85 DEG C of isothermal reaction 3～3.5h, add the Halogen group elements monomer of the amount half being equivalent to pyridines monomeric substance, water
Bath is warming up to 94～99 DEG C, continues stirring reaction 2 hours, is slowly cooled to room temperature, and obtains compound alkyl pyridine quaternary ammonium salt；
S2, the synthesis of corrosion inhibiter: the fatty alcohol-polyoxyethylene ether of 4%～8wt% is added having to 25%～30wt%
In machine acid, stir to making it be completely dissolved, form homogeneous mixing liquid i；Then sequentially add surplus in mixing liquid i
Water, the Organic Alcohol of 5%～10wt%, the alkynol of 2%～5wt%, the organic aldehyde of 4%～8wt%, stir to making its mix homogeneously
Obtain mixing liquid ii；The compound alkylated pyrazole preparing through step s1 of 18%～30wt% is added in the most backward mixing liquid ii
Pyridine quaternary ammonium salt, continues stirring 0.5～1h so as to uniform mix, that is, obtains high temperature resistant acidification corrosion inhibitor.
This is high temperature resistant, and acidification corrosion inhibitor dosage when using is generally 1.5～2.5wt%.
Compared with prior art, this resistance to 140～160 DEG C of high temperature acidified use corrosion inhibiter good dispersion, compatibilities in acid solution
Good, coking few it is adaptable to deep-well acid stimulation job execution；Its consumption be only 2% in the case of, corrosion rate≤20g/
(m2H), far superior to industry primes standard, corrosion mitigating effect is very good；Additionally, this resistance to 140 DEG C～160 DEG C high temperature acidified use
Corrosion inhibiter is easy to get from raw material, and reaction condition is gentle, simple production process；It can be seen that, this is high temperature resistant, and corrosion inhibiter maximum limit is used in acidifying
Degree ground reduces the corrosion to equipment and tubing string for the acid solution it is ensured that high temperature acidified construction is smoothed out.
Specific embodiment
With reference to specific embodiment, the present invention is described further, but following embodiment absolutely not the present invention is had appoint
What limits.
Embodiment 1
1) it is combined the synthesis of pyridine quaternary ammonium salt: 2,6- lutidines, 3- picoline, benzyl chloride are pressed the amount ratio of material
It is completely dissolved in the mixed solution of alcohol-water (volume ratio 1:1) for 1:1:2.1 ratio, after 80 DEG C of isothermal reactions 3 hours, then
Add the benzyl chloride with amounts of material such as 2,6- lutidines, warming-in-water, to 95 DEG C, continues stirring reaction 2 hours, slowly
It is cooled to room temperature, obtain compound alkyl pyridine quaternary ammonium salt；
2) high temperature resistant acidification corrosion inhibitor preparation: 4 weight portion aeo-9 are added in 25 weight portion formic acid, are stirred, make
It is completely dissolved, and forms homogeneous mixing liquid i；Then 40 weight portion water, 5 weight portion second two are added successively in mixing liquid i
Alcohol, the tertiary alkynol of 2 weight portions and 4 parts by weight of formaldehyde, continuing stirring makes its mix homogeneously；It is eventually adding the compound alkyl of 20 weight portions
Pyridine quaternary ammonium salt, stir about half an hour so as to uniform mix, that is, obtains 140～160 DEG C of high-temperature acidification corrosion inhibitor a of heatproof.
Embodiment 2
1) it is combined the synthesis of pyridine quaternary ammonium salt: 2,3,5- trimethylpyridine, 2,4- lutidines, 1 chloromethyl naphthalene are pressed
The amount of material is completely dissolved in the mixed solution of alcohol-water (volume ratio 1:1) than for 1:1:2.4 ratio, 85 DEG C of isothermal reactions 3
After hour, add the 1 chloromethyl naphthalene with amounts of material such as 2,3,5- trimethylpyridines, warming-in-water, to 95 DEG C, continues stirring
Reaction 2 hours, is slowly cooled to room temperature, and obtains compound alkyl pyridine quaternary ammonium salt；
2) high temperature resistant acidification corrosion inhibitor preparation: 6 weight portion aeo-15 are added in 28 weight portion formic acid, are stirred,
So that it is completely dissolved, form homogeneous mixing liquid i；Then 24 weight portion water, 8 weight portion second are added successively in mixing liquid i
Glycol, 3 weight portion propilolic alcohols and 6 weight portion cinnamic aldehydes, continuing stirring makes its mix homogeneously；It is eventually adding the compound of 25 weight portions
Alkyl pyridine quaternary ammonium salt, stir about half an hour so as to uniform mix, that is, obtains 140～160 DEG C of high-temperature acidification corrosion inhibitor b of heatproof.
Embodiment 3
1) it is combined the synthesis of pyridine quaternary ammonium salt: 2,3,5- trimethylpyridine, 2,4- lutidines, 1 chloromethyl naphthalene are pressed
The amount of material is completely dissolved in the mixed solution of alcohol-water (volume ratio 1:1) than for 1:1:2.4 ratio, 85 DEG C of isothermal reactions 3
After hour, add the 1 chloromethyl naphthalene with amounts of material such as 2,3,5- trimethylpyridines, warming-in-water, to 95 DEG C, continues stirring
Reaction 2 hours, is slowly cooled to room temperature, and obtains compound alkyl pyridine quaternary ammonium salt；
2) high temperature resistant acidification corrosion inhibitor preparation: 8 weight portion aeo-20 are added in 30 weight portion formic acid, are stirred,
So that it is completely dissolved, form homogeneous mixing liquid i；Then 10 weight portion water, 10 weight portion second are added successively in mixing liquid i
Glycol, 4 weight portion propilolic alcohols and 8 weight portion cinnamic aldehydes, continuing stirring makes its mix homogeneously；It is eventually adding the compound of 30 weight portions
Alkyl pyridine quaternary ammonium salt, stir about half an hour so as to uniform mix, that is, obtains 140～160 DEG C of high-temperature acidification corrosion inhibitor c of heatproof.
Performance test:
(1) according to People's Republic of China's oil and gas industry standard " sy/t5405-1996 " method, to embodiment 1
The corrosion inhibiter sample of～3 preparations has carried out corrosion inhibition test, and concrete test result see table 1.
Table 1:
From table 1 it follows that corrosion inhibitor product a, b of embodiment 1～3 preparation and c dosage are in 1.5～2.5% scopes
Interior, all show good corrosion mitigating effect at 140～160 DEG C, and good dispersion, compatibility are good in acid solution.
(2) above-mentioned corrosion inhibiter site operation application example:
Ordovician Buried Hills oil-gas reservoir be Nanpu Oilfield main force's oil and gas bearing series, buried hill fissure, hole develop, be hole-
Crack elimination, crack major developmental build joint and seam, but be filled with, only minority late period build joint is unfilled. more
Belong to special low hole, special hypotonic type reservoir, and reservoir oil-containing is uneven.
Wherein, certain well is positioned at a bite horizontal well in this structural high part, and its finishing drilling well depth is 5000m, using bore hole
Completion mode completion, open-hole interval length is 260m, and lithology is taupe gray limestone, taupe gray argillaceous limestone, and interval of interest is logged well
Be construed to, class low permeability reservoir, fracture development, and no obvious oil/gas show when testing.From known block offset well test data
See, reservoir pressure coefficient 1.0, normally, 160 DEG C of predicted temperature.
Resistance to 160 DEG C of high-temperature corrosion inhibitor product c using embodiment 3 preparation；Acid fluid system is: 20% hydrochloric acid+0.5bz acidifying
With gellant+2% ferrous stability+2% cleanup additive+2% clay stabilizer, it is satisfied by 160 DEG C of construction requirements；For ensureing acid
After pressure transformation, reservoir has higher flow conductivity, using the compound acid fracturing work of " preposition+multistage injection+steering+closure " in technique
Skill technology is constructed.
This well smoothly completes acid fracturing construction, and construct max. pump pressure 55mpa, and highest discharge capacity is 4.3m3/ min, open flow after acid fracturing
Discharge opeing, after open flow, oil pressure rises comparatively fast, once lights a fire successfully after 10h, oil nozzle 5mm, oil pressure 25mpa, and conversion gas production is
28890m3/ d, transformation achieves good effect.
Claims (8)
1. a kind of resistance to 140 DEG C～160 DEG C high temperature acidified use corrosion inhibiter are it is characterised in that include the component of following mass fraction:
2. resistance to 140 DEG C～160 DEG C high temperature acidified use corrosion inhibiter according to claim 1 are it is characterised in that described compound alkane
Yl pyridines quaternary ammonium salt passes through:
2,3,5- trimethylpyridine, 2,4- lutidines and 1 chloromethyl naphthalene press the amount of material ratio for 1:1:(3.0～3.5) anti-
Should generate；
Or 2,4,6- trimethylpyridine, 2,5- lutidines and 2- bromomethyl naphthalene press the amount of material than for 1:1:(3.0～3.5)
Reaction generates；
Or 2,6- lutidines, 3- picoline and benzyl chloride press the amount of material ratio for 1:1:(3.0～3.5) reaction generates.
3. resistance to 140 DEG C～160 DEG C high temperature acidified use corrosion inhibiter according to claim 1 are it is characterised in that described fatty alcohol
Polyoxyethylene ether is aeo-9, aeo-15 or aeo-20.
4. resistance to 140 DEG C～160 DEG C high temperature acidified use corrosion inhibiter according to claim 1 are it is characterised in that described organic aldehyde
For formaldehyde, paraformaldehyde, acetaldehyde or cinnamic aldehyde.
5. resistance to 140 DEG C～160 DEG C high temperature acidified use corrosion inhibiter according to claim 1 are it is characterised in that described alkynol third
Alkynol, methyl butynol, methylparafynol, tertiary alkynol or dimethylated hexynol.
6. resistance to 140 DEG C～160 DEG C high temperature acidified use corrosion inhibiter according to claim 1 are it is characterised in that described organic acid
For formic acid or acetic acid.
7. resistance to 140 DEG C～160 DEG C high temperature acidified use corrosion inhibiter according to claim 1 are it is characterised in that described Organic Alcohol
For ethanol, isobutanol or ethylene glycol.
8. a kind of preparation method preparing high temperature resistant acidifying corrosion inhibiter is it is characterised in that comprise the steps:
S1, the synthesis of compound pyridine quaternary ammonium salt: pyridines monomer and Halogen group elements monomer are pressed the amount of material ratio for 2:(2.0
～2.5) ratio is completely dissolved in ethanol-water solution (vWater:vAlcohol=1:1) in, after 80～85 DEG C of isothermal reaction 3～3.5h, then plus
Enter to be equivalent to the Halogen group elements monomer of the amount half of pyridines monomeric substance, warming-in-water, to 94～99 DEG C, continues stirring anti-
Answer 2～2.5h, be slowly cooled to room temperature, obtain compound alkyl pyridine quaternary ammonium salt；
S2, the synthesis of corrosion inhibiter: fatty alcohol-polyoxyethylene ether is added to organic acid, stirs to making it be completely dissolved, formed
Homogeneous mixing liquid i；Then sequentially add water, Organic Alcohol, alkynol, organic aldehyde in mixing liquid i, stir to making it mix all
Even obtain mixing liquid ii；Add the compound alkyl pyridine quaternary ammonium salt preparing through step s1 in the most backward mixing liquid ii, continue
Continuous stirring 0.5～1h so as to uniform mix, that is, obtains high temperature resistant acidification corrosion inhibitor.
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Cited By (11)
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| CN107418547A (en) * | 2017-08-29 | 2017-12-01 | 中国石油集团渤海钻探工程有限公司 | One kind is based on the high-temperature acidification corrosion inhibitor of tribenzyl (2 benzyl) pyridine ammonium chloride |
| CN107523287A (en) * | 2017-08-29 | 2017-12-29 | 中国石油集团渤海钻探工程有限公司 | A kind of combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt |
| CN108264891A (en) * | 2017-12-29 | 2018-07-10 | 南京华洲新材料有限公司 | A kind of oil-soluble inhibitor and preparation method thereof |
| CN110129022A (en) * | 2019-04-19 | 2019-08-16 | 中国石油天然气股份有限公司 | High-temperature-resistant corrosion inhibitor for online acidification and preparation and use methods thereof |
| CN110229377A (en) * | 2019-06-28 | 2019-09-13 | 濮阳班德路化学有限公司 | A kind of dechlorination method of light dydrocarbon solvent |
| CN112226220A (en) * | 2020-09-29 | 2021-01-15 | 陈力群 | High-temperature acidizing corrosion inhibitor and preparation method thereof |
| CN112442348A (en) * | 2020-12-17 | 2021-03-05 | 西安文理学院 | Acidizing corrosion inhibitor for acidizing and plugging removal and preparation method thereof |
| CN114481137A (en) * | 2021-12-21 | 2022-05-13 | 宜兴汉光高新石化有限公司 | Additive for retarding corrosion of high-temperature organic acid and preparation method thereof |
| CN114591224A (en) * | 2020-12-03 | 2022-06-07 | 中国石油天然气股份有限公司 | Corrosion inhibitor with hydrate inhibition function and preparation method and application thereof |
| US20220333002A1 (en) * | 2021-04-20 | 2022-10-20 | Saudi Arabian Oil Company | Acid corrosion inhibitors |
| CN117448821A (en) * | 2023-10-30 | 2024-01-26 | 中国石油大学(华东) | Composite acidizing corrosion inhibitor compound based on indolizine derivative and preparation method thereof |
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Cited By (18)
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| CN107523287A (en) * | 2017-08-29 | 2017-12-29 | 中国石油集团渤海钻探工程有限公司 | A kind of combined high temperature acidification corrosion inhibitor based on pyridines quaternary ammonium salt |
| CN107418547A (en) * | 2017-08-29 | 2017-12-01 | 中国石油集团渤海钻探工程有限公司 | One kind is based on the high-temperature acidification corrosion inhibitor of tribenzyl (2 benzyl) pyridine ammonium chloride |
| CN108264891A (en) * | 2017-12-29 | 2018-07-10 | 南京华洲新材料有限公司 | A kind of oil-soluble inhibitor and preparation method thereof |
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Application publication date: 20170201 |