CN102676140A - Nitrogenous heterocyclic quaternary ammonium salt acidizing corrosion inhibitor and preparation method thereof - Google Patents
Nitrogenous heterocyclic quaternary ammonium salt acidizing corrosion inhibitor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nitrogenous heterocyclic quaternary ammonium salt acidizing corrosion inhibitor and a preparation method thereof. The nitrogenous heterocyclic quaternary ammonium salt acidizing corrosion inhibitor comprises the following components in percentage by weight: component 1, propargyl alcohol, formaldehyde, urotropine, potassium iodide, antimonous oxide, antimony butter, surfactant and solvent in the ratio of (1-50) : (0-25) : (1-25) : (0-10) :(0-10) : (0-20) : (6-25) : (15-70), wherein the component 1 is selected from one or more of chlorinated N-benzyl-R-pyridine quaternary ammonium salt or chlorinated N-benzyl-R-quinoline quaternary ammonium salt. The nitrogenous heterocyclic quaternary ammonium salt acidizing corrosion inhibitor has the advantages of small addition amount, low cost, stable and uniform dispersion in acidic liquid, low corrosion speed, capability of resisting high temperature of over 160 DEG C and excellent performance. 0.5-2.5 percent of nitrogenous heterocyclic quaternary ammonium salt acidizing corrosion inhibitor disclosed by the invention is added into the acidic liquid, so that the corrosion speed is far lower than national primary standard.
Description
Technical field
The invention belongs to the anticorrosive metal technical field, relate to a kind of nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor and preparation method thereof.
Background technology
Acidification technology of oil well is claimed acid treatment process again, is meant to adopt mechanical means that a certain amount of acid solution is injected into the stratum from ground through oil well, because the solvable obstruction material of taking off near the stratum, shaft bottom of acid solution; Like the mud tamper; Some component in the corrosion formation rock makes formation pore and crack enlarge, link up, and the in-place oil circulation road increases; The in-place oil resistance to flow descends, thereby reaches the purpose of raising the output.Yet acid solution all has stronger corrodibility to metal pipe line equipment and downhole oil tubing string, and accidents such as impaired, the downhole oil tubing string heavy corrosion of acidizing unit and the oil pipe of threading off on the normal spot have had a strong impact on the ordinary production of crude oil.
Inhibiter is a kind ofly to be present in the environment (medium) with suitable concentration and form, prevents and slow down the mixture of corrosive chemical substance or several kinds of chemical substances.Consumption is few, construction technology is easy owing to having for inhibiter, do not need special optional equipment advantages such as (like electro-chemical protections) to enjoy liking of people.In the acidizing treatment process, rely on exactly in the acid solution and to add acidification corrosion inhibitor and suppress the corrosion of acid solution down-hole string.
Along with the development of drilling technology and the progress of oil recovery technique, a large amount of deep-wells, ultra deep well (more than 7000 meters) and profound well (more than 15000 meters) drop into exploitation, and the acidifying measure increases year by year, and is also higher with the performance requirement of inhibiter to acidifying.Research and develop out that to be used for FT more than 160 ℃, low injury, resistant to elevated temperatures acidification corrosion inhibitor more and more urgent.High-temperature corrosion inhibitor commonly used both at home and abroad now is at the high temperature concentrated acid (more than 160 ℃; 20%HCL) be prone to big, the shortcomings such as cost is high, the Oil Tube Steel corrosion speed big, inhibition efficiency difference of coking, layering, dissolution dispersity add-on stable inadequately, inhibiter in the environment; Also possibly in the stratum, be formed into the shallow lake in addition, cause formation damage.
Therefore, urgently on the market be badly in need of that a kind of addition is few, with low cost, stable and uniform is disperseed in acid solution, corrosion speed is little, can be anti-the oil gas well high-temperature acidification corrosion inhibitor of high temperature, excellent property more than 160 ℃.
Summary of the invention
The objective of the invention is above-mentioned defective, a kind of nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor is provided to prior art.
Another object of the present invention provides the preparation method of this nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor.
The object of the invention can be realized through following technical scheme:
A kind of nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor contains following components in part by weight: component 1: propiolic alcohol: formaldehyde: urotropine: potassiumiodide: Antimony Trioxide: 99.5Min: butter of antimony: tensio-active agent: solvent=(1～50): (0～25): (1～25): (0～10): (0～10): (0～20): (0～20): (6～25): (15～70); Wherein said component 1 is selected from one or more in chlorination N-benzyl-R-pyridine quaternary ammonium salt or the chlorination-N-benzyl-R-quinoline quaternary ammonium salt.
Described chlorination N-benzyl-R-pyridine quaternary ammonium salt prepares through following method: one or more in the mixture of the pyridine derivate that Benzyl Chloride and pyridine, pyridine derivate or still are residual reacted 3～8 hours down at 120 ℃～180 ℃, made described chlorination N-benzyl-R-pyridine quaternary ammonium salt; Wherein, the weight ratio of one or more in the mixture of Benzyl Chloride and pyridine, pyridine derivate or pyridine derivate is 1: (1～1.5).
Described pyridine derivate is selected from 2-picoline, 4-picoline, 2,3 dimethyl pyridine, 2,4-lutidine, 2,5-lutidine; 2,6-lutidine, 3,4-lutidine, 3,5-lutidine; 2,2,3, the 5-trimethylpyridine.
The mixture of the pyridine derivate that described still is residual is the cut more than 180 ℃ of intercepting coal tar or pyridine synthesis.
Described chlorination-N-benzyl-R-quinoline quaternary ammonium salt prepares through following method: Benzyl Chloride and technical quinoline reacted 3～8 hours down at 130 ℃～180 ℃, made described chlorination N-benzyl-R-quinoline quaternary ammonium salt; Wherein, the weight ratio of Benzyl Chloride technical quinoline is 1: (1～1.8).
Described tensio-active agent is selected from O-15, O-25, OP-10, OP-8.
Described solvent is selected from methyl alcohol, ethanol, Virahol or its mixture.
The preparation method of nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor of the present invention comprises following steps:
(1) preparation chlorination N-benzyl-R-pyridine quaternary ammonium salt: one or more in the mixture of the pyridine derivate that Benzyl Chloride and pyridine, pyridine derivate or still are residual reacted 3～8 hours down at 120 ℃～180 ℃, made described chlorination N-benzyl-R-pyridine quaternary ammonium salt; Wherein, the weight ratio of the mixture of Benzyl Chloride and pyridine or pyridine derivate or pyridine derivate is 1: (1～1.5); Perhaps, preparation chlorination-N-benzyl-R-quinoline quaternary ammonium salt: Benzyl Chloride and technical quinoline reacted 3～8 hours down at 130 ℃～180 ℃, made described chlorination N-benzyl-R-quinoline quaternary ammonium salt; Wherein, the weight ratio of Benzyl Chloride technical quinoline is 1: (1～1.8);
(2) get in chlorination N-benzyl-R-pyridine quaternary ammonium salt or chlorination-N-benzyl-R-quinoline quaternary ammonium salt one or more as component 1, and propiolic alcohol: formaldehyde: urotropine: potassiumiodide: Antimony Trioxide: 99.5Min: butter of antimony: tensio-active agent: solvent is mixed with according to following weight ratio and obtains described nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor: component 1: propiolic alcohol: formaldehyde: urotropine: potassiumiodide: Antimony Trioxide: 99.5Min: butter of antimony: tensio-active agent: solvent=(1～50): (0～25): (1～25): (0～10): (0～10): (0～20): (0～20): (6～25): (15～70).
Described pyridine derivate is selected from 2-picoline, 4-picoline, 2,3 dimethyl pyridine, 2,4-lutidine, 2,5-lutidine; 2,6-lutidine, 3,4-lutidine, 3,5-lutidine; 2,2,3, the 5-trimethylpyridine; The mixture of the pyridine derivate that described still is residual is intercepting coal tar or the cut of industrial pyridine synthesis still more than 180 ℃; Described tensio-active agent is selected from O-15, O-25, OP-10, OP-8; Described solvent is selected from methyl alcohol, ethanol, Virahol or its mixture.
Beneficial effect:
The present invention is directed in the prior art high-temperature corrosion inhibitor at the high temperature concentrated acid (more than 160 ℃; 20%HCL) be prone to big, the shortcomings such as cost is high, the Oil Tube Steel corrosion speed big, inhibition efficiency difference of coking, layering, dissolution dispersity add-on stable inadequately, inhibiter in the environment, a kind of novel azaheterocyclic class quaternary ammonium salt acidification corrosion inhibitor is provided.This buffer reagent addition is few, with low cost, stable and uniform is disperseed in acid solution, corrosion speed is little, can be anti-high temperature, excellent property more than 160 ℃.In acid solution, add 0.5%～2.5% (wt) nitrogen heterocyclic ring class of the present invention quaternary ammonium salt acidification corrosion inhibitor, can make erosion rate far below country-level standard.
The method of this high temperature nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor of preparation provided by the invention; Wherein the raw material sources of important component are extensive, synthetic route is simple; Synthesis condition is not harsh; Make the preparation cost of nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor significantly reduce large-scale commercial prodn preferably and application.
Embodiment
Embodiment 1
The residual cut more than 180 ℃ of industrial pyridine synthesis still adds in the reaction kettle according to 1: 1 ratio of weight ratio under Benzyl Chloride and the normal pressure, reacts 4 hours down at 160 ℃, makes chlorination N-benzyl-R-pyridine quaternary ammonium salt; The chlorination N-benzyl-R pyridine quaternary ammonium salt of preparation, propiolic alcohol, formaldehyde, potassiumiodide, butter of antimony, O-15, methyl alcohol were by weight 40: 5: 5: 1: 15: 15: 19, obtain inhibiter A after stirring.
Embodiment 2
Benzyl Chloride, technical quinoline add in the reaction kettle according to 1: 1 ratio of weight ratio, react 4 hours down at 160 ℃, make chlorination N-benzyl-R-quinoline quaternary ammonium salt; The chlorination N-benzyl-R-quinoline quaternary ammonium salt, propiolic alcohol, formaldehyde, potassiumiodide, Antimony Trioxide: 99.5Min, O-15, methyl alcohol of preparation is by weight being 40: 5: 5: 1: 15: 15: 19, obtain inhibiter B after stirring.
Embodiment 3
Get among embodiment 1 and the embodiment 2 and make chlorination N-benzyl-R pyridine quaternary ammonium salt and chlorination N-benzyl-R-quinoline quaternary ammonium salt; Chlorination N-benzyl-R-pyridine quaternary ammonium salt (embodiment 1 preparation), chlorination N-benzyl-R-quinoline quaternary ammonium salt (embodiment 2 preparations), propiolic alcohol, formaldehyde, potassiumiodide, Antimony Trioxide: 99.5Min, O-15, methyl alcohol are by weight being 20: 20: 5: 5: 1: 15: 15: 19, obtain inhibiter C after stirring.
Embodiment 4
Benzyl Chloride and 2-picoline, 4-picoline; 2,3 dimethyl pyridine and 2, the mixture of 4-lutidine (2-picoline: 4-picoline: 2; 3-lutidine: 2; The mass ratio of 4-lutidine 1: 1: 1: 1) add in the reaction kettle, reacted 4 hours down, make chlorination N-benzyl-R-pyridine quaternary ammonium salt at 160 ℃ according to 1: 1.5 ratio of weight ratio; The chlorination N-benzyl-R pyridine quaternary ammonium salt of preparation, propiolic alcohol, formaldehyde, potassiumiodide, butter of antimony, OP-8, methyl alcohol were by weight 45: 10: 15: 5: 10: 10: 30, obtain inhibiter D after stirring.
Embodiment 5
Benzyl Chloride and 2,5-lutidine, 3, the mixture (2 of 5-lutidine; 5-lutidine: 3; The mass ratio of 5-lutidine 2: 1) adds in the reaction kettle according to 1: 1.2 ratio of weight ratio, reacted 4 hours down, make chlorination N-benzyl-R-pyridine quaternary ammonium salt at 160 ℃; The chlorination N-benzyl-R pyridine quaternary ammonium salt of preparation, propiolic alcohol, formaldehyde, urotropine, potassiumiodide, tri-chlorination two antimony, butter of antimony, OP-10, methyl alcohol were by weight 35: 25: 10: 9: 8: 10: 10: 20: 50, obtain inhibiter E after stirring.
Embodiment 6
In order to check corrosion mitigating effect of the present invention, get the foregoing description 1～5 resulting buffer reagent product, according to standard SY-T5405-1996 " acidifying is with inhibiter method for testing performance and evaluation index " its corrosion inhibition is estimated, the result is following:
Lose speed all far below national standard, and at high temperature seldom have coking phenomenon to take place.
More than be that the technical scheme that the embodiment of the invention is provided has been carried out detailed introduction; Use a concrete example among this paper and only be embodiment of the invention principle and elaboration that embodiment carried out, the explanation of above embodiment only is applicable to that help understands the principle of the embodiment of the invention; Simultaneously, for one of ordinary skill in the art, according to the embodiment of the invention, the part that on embodiment and range of application, all can change, in sum, this description should not be construed as limitation of the present invention.
Claims (9)
1. a nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor is characterized in that containing following components in part by weight: component 1: propiolic alcohol: formaldehyde: urotropine: potassiumiodide: Antimony Trioxide: 99.5Min: butter of antimony: tensio-active agent: solvent=(1～50): (0～25): (1～25): (0～10): (0～10): (0～20): (0～20): (6～25): (15～70); Wherein said component 1 is selected from one or more in chlorination N-benzyl-R-pyridine quaternary ammonium salt or the chlorination-N-benzyl-R-quinoline quaternary ammonium salt.
2. nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor according to claim 1; It is characterized in that described chlorination N-benzyl-R-pyridine quaternary ammonium salt prepares through following method: one or more in the mixture of the pyridine derivate that Benzyl Chloride and pyridine, pyridine derivate or still are residual reacted 3～8 hours down at 120 ℃～180 ℃, made described chlorination N-benzyl-R-pyridine quaternary ammonium salt; Wherein, the weight ratio of one or more in the mixture of Benzyl Chloride and pyridine, pyridine derivate or pyridine derivate is 1: (1～1.5).
3. nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor according to claim 2 is characterized in that described pyridine derivate is selected from 2-picoline, 4-picoline, 2,3 dimethyl pyridine, 2; The 4-lutidine, 2,5-lutidine, 2,6-lutidine; 3,4-lutidine, 3,5-lutidine, 2; 4,6-trimethylpyridine, 2,3,5-trimethylpyridine.
4. nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor according to claim 2, the mixture that it is characterized in that the pyridine derivate that described still is residual are intercepting coal tar or the cut of industrial pyridine synthesis still more than 180 ℃.
5. nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor according to claim 1; It is characterized in that described chlorination-N-benzyl-R-quinoline quaternary ammonium salt prepares through following method: Benzyl Chloride and technical quinoline reacted 3～8 hours down at 130 ℃～180 ℃, made described chlorination N-benzyl-R-quinoline quaternary ammonium salt; Wherein, the weight ratio of Benzyl Chloride technical quinoline is 1: (1～1.8).
6. nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor according to claim 1 is characterized in that described tensio-active agent is selected from O-15, O-25, OP-10, OP-8.
7. nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor according to claim 1 is characterized in that described solvent is selected from methyl alcohol, ethanol, Virahol or its mixture.
8. the preparation method of the described nitrogen heterocyclic ring class of claim 1 quaternary ammonium salt acidification corrosion inhibitor is characterized in that comprising following steps:
(1) preparation chlorination N-benzyl-R-pyridine quaternary ammonium salt: one or more in the mixture of the pyridine derivate that Benzyl Chloride and pyridine, pyridine derivate or still are residual reacted 3～8 hours down at 120 ℃～180 ℃, made described chlorination N-benzyl-R-pyridine quaternary ammonium salt; Wherein, the weight ratio of the mixture of Benzyl Chloride and pyridine or pyridine derivate or pyridine derivate is 1: (1～1.5); Perhaps, preparation chlorination-N-benzyl-R-quinoline quaternary ammonium salt: Benzyl Chloride and technical quinoline reacted 3～8 hours down at 130 ℃～180 ℃, made described chlorination N-benzyl-R-quinoline quaternary ammonium salt; Wherein, the weight ratio of Benzyl Chloride technical quinoline is 1: (1～1.8);
(2) get in chlorination N-benzyl-R-pyridine quaternary ammonium salt or chlorination-N-benzyl-R-quinoline quaternary ammonium salt one or more as component 1, and propiolic alcohol: formaldehyde: urotropine: potassiumiodide: Antimony Trioxide: 99.5Min: butter of antimony: tensio-active agent: solvent is mixed with according to following weight ratio and obtains described nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor: component 1: propiolic alcohol: formaldehyde: urotropine: potassiumiodide: Antimony Trioxide: 99.5Min: butter of antimony: tensio-active agent: solvent=(1～50): (0～25): (1～25): (0～10): (0～10): (0～20): (0～20): (6～25): (15～70).
9. the preparation method of nitrogen heterocyclic ring class quaternary ammonium salt acidification corrosion inhibitor according to claim 8 is characterized in that described pyridine derivate is selected from 2-picoline, 4-picoline, 2,3 dimethyl pyridine, 2; The 4-lutidine, 2,5-lutidine, 2,6-lutidine; 3,4-lutidine, 3,5-lutidine, 2; 4,6-trimethylpyridine, 2,3,5-trimethylpyridine; The mixture of the pyridine derivate that described still is residual is intercepting coal tar or the cut of industrial pyridine synthesis still more than 180 ℃; Described tensio-active agent is selected from O-15, O-25, OP-10, OP-8; Described solvent is selected from methyl alcohol, ethanol, Virahol or its mixture.
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