CN1584121A - Inhibitor, preparing method and use thereof - Google Patents

Inhibitor, preparing method and use thereof Download PDF

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Publication number
CN1584121A
CN1584121A CN 200410010318 CN200410010318A CN1584121A CN 1584121 A CN1584121 A CN 1584121A CN 200410010318 CN200410010318 CN 200410010318 CN 200410010318 A CN200410010318 A CN 200410010318A CN 1584121 A CN1584121 A CN 1584121A
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Prior art keywords
inhibitor
acid
carboxylic acid
preparation
inhibiter
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CN1283838C (en
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王菁辉
杨金辉
郭鹏
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Sinopec Luoyang Guangzhou Engineering Co Ltd
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Sinopec Luoyang Petrochemical Engineering Corp
China Petrochemical Corp
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Abstract

An inhibitor, its preparing method and use are disclosed. It consists of corrosion inhibitor 90-97wt% and anticorrosion improver 3-10wt%. The R is linear or branched paraffin or olefine containing 8-10 carbon atomic, the n1 is 0-4 integer, the anticorrosion improver is organic acid zinc salt or inorganic acid zinc salt. The inhibitor is used by adding the 5-150mg/L inhibitor into system containing H2S-H2O. Its advantages include high-temperature and pH value resistant performance, and good solubility and dispersion.

Description

A kind of inhibitor and its production and application
Technical field
The invention belongs to the metal material surface anticorrosion technique, particularly relate to a kind of inhibitor and its production and application.
Background technology
Along with the deterioration of domestic crude oil and the increase of import high-sulfur crude oil, the etching problem of Petrochemical Enterprises is serious day by day, making originally is not that the etching problem at key protection position more and more causes concern, as condensation cooling system, LPG cyoinders, liquid hydrocarbon storage tank and the hydrogenation unit etc. of desulfurizer regenerator column.The corrosion of this class device mainly is CO 2-H 2S-H 2O, H 2S-H 2The O corrosion.Steel produces corrosion such as general corrosion, hydrogen bulge, sulfide-stress cracking under this environment.For this type of corrosion, generally solve by two kinds of approach both at home and abroad: a kind of is raising equipment material rate; Another kind is to solve etching problem by the technology protection.
And for existing installation can only adopting process the measure of protection solve etching problem, simple effective method is annotated inhibiter exactly.The inhibiter kind of present domestic use is a lot, and patent is also a lot, discloses a kind of novel refinery oil-soluble inhibitor as CN1091781A, and CN1144856C discloses a kind of oil field novel anti CO 2Corrosion inhibitor, CN1144857C disclose a kind of oil field water filling inhibiter, and CN1410595A discloses a kind of inhibition carbon steel CO 2Corrosive water soluble rust inhibitor and preparation method thereof, CN1422984A disclose a kind of metal inhibitor.Wherein among CN1144856C, CN1144857C and the CN1410595A disclosed inhibiter can be in certain temperature, contain CO 2High salinity sewage environment in metallic conduit and equipment are effectively protected, can be applicable to and contain CO 2In the oil well, mainly be at CO 2Corrosion.And disclosed inhibiter is at the refinery HCl-H that often reduces pressure among CN1091781A and the CN1422984A 2S-H 2O type corrosive medium, main corrosion is that HCl produces in this medium since at corrosive medium and corrosive environment different, so the inhibiter in these patents is unsuitable for being applied in H from principle 2S-H 2In the O corrosive medium, practical application effect is also bad.
External inhibiter such as U.S. Pat P4404167, USP5151220 and the USP0020001536 etc. that use.Wherein limited, the easy emulsification of the solvability of disclosed inhibiter in water among the USP4404167, use inconvenience; Disclosed inhibiter is an oil-soluble inhibitor among the USP5151220, usage quantity is less, suppresses efficient and reaches 95%, but exist using dosage poorly to grasp, the injection rate surface of equipment and pipeline too hour in the back forms the successive protective membrane, and injection rate has the possibility of pollution medium greatly again; Disclosed inhibiter is to be used for particular environment among the USP0020001536, suppress the corrosion of alkyl group hydramine, hot carbonate solution, diglyme and other solvent gas system, the corrosion of the equipment that inhibition and amine-based solvents and sour gas such as hydrogen sulfide, carbonic acid gas contact is unsuitable for H 2S-H 2The O system.
Summary of the invention
The present invention is in order to solve in the prior art not at H 2S-H 2Suitable inhibitor in the O corrosive environment, a kind of novel inhibitor is provided, film-forming properties, the temperature tolerance of the existing oil soluble inhibitor of this inhibitor, be difficult for emulsification, and adapt to the characteristics such as variation of pH value, water-soluble inhibitor good solubility, dispersiveness are arranged again.
The present invention also provides a kind of preparation method and the application of this inhibitor in addition.
Inhibitor provided by the invention is made up of the inhibiter of 90-97 weight % and the protection against corrosion promotor of 3-10 weight %.
Wherein the general structure of inhibiter is as the formula (1):
Figure A20041001031800051
R has 8～30 carbon atoms in the formula, the preferably straight chain of 12～24 carbon atoms or branched alkyl or alkylene, cycloalkyl group or cycloalkenyl group, and the structural formula of R ' is Wherein n1 is 0～4 integer.
Protection against corrosion promotor is organic acid zinc salt or mineral acid zinc salt, as zinc sulfate, zinc nitrate, zinc acetate, Zinc Gluconate etc., preferably zinc sulfate.
The present invention also provides the preparation method of this inhibitor, and the step of this method is as follows:
I) preparation inhibiter
(a) organic acid and polyethylene polyamine are 1～5: 5～1 mixing in molar ratio, 5～30% the azeotropic agent that adds reactant weight then, be warmed up to 140-160 ℃, constant temperature 1～10 hour, be warmed up to 200～240 ℃ with 10 ℃ speed per hour then, constant temperature 3～10 hours makes binary system be condensed into the oil-soluble intermediate that contains the bicyclic imidazo quinoline.
Wherein said organic acid is aliphatic carboxylic acid, alicyclic carboxylic acid or their mixture.
Aliphatic carboxylic acid has 8～30 carbon atoms, and preferably 12～24 carbon atoms can be straight chains, also can have side chain; Can be saturated, also can be undersaturated; Aliphatic carboxylic acid is recommended to use monoprotic acid or diprotic acid preferably, as oleic acid, linolic acid, stearic acid or dodecenylsuccinic acid etc.
Alicyclic carboxylic acid is that molecular-weight average is 240～500, is preferably 260～300, has the carboxylic acid of 1～5 ring, and wherein Huan carbonatoms is recommended as 5 or 6, is preferably 5; This alicyclic carboxylic acid is monoprotic acid preferably.
Azeotropic agent is an aromatic hydrocarbon solvent, and preferred mononuclear aromatics solvent is as toluene, dimethylbenzene or their mixture.
The structural formula of polyethylene polyamine is H 2N (CH 2CH 2NH) N2CH 2CH 2NH 2, wherein n2 is 2～6 integer.Polyethylene polyamine recommends to use triethylene tetramine, tetraethylene pentamine, five ethene hexamines or their mixture.
(b) add solubility promoter in step (a) gained intermediate, under agitation condition, slowly add transforming agent, whole dropping and reaction times are 1～3 hour, make it to be converted into inhibiter.
Wherein said solubility promoter is the Fatty Alcohol(C12-C14 and C12-C18) that 2～4 carbon atoms are arranged, and recommends to use ethanol, propyl alcohol, Virahol or butanols etc., and usage quantity is 20～100% of an intermediate weight.
Transforming agent is the aliphatic carboxylic acid that 1～4 carbon atom is arranged, and as formic acid, acetate or vinylformic acid etc., usage quantity is 20～50% of an intermediate weight, also can determine usage quantity according to the system pH value, when the pH value of whole system 7～8 the time, can stop to drip.
II) preparation inhibitor
With step I) in the preparation inhibiter and protection against corrosion promotor composite at normal temperatures and pressures, obtain inhibitor of the present invention.
Inhibitor provided by the present invention can be used for containing H 2S-H 2The system of O particularly can be used for condensation cooling system, LPG cyoinders, liquid hydrocarbon storage tank and the hydrogenation unit etc. of the regenerator column of desulfurizer, during use inhibitor of the present invention is joined with the consumption of 5～150mg/L and contains H 2S-H 2In the system of O.
The present invention is compared with prior art with strong points, and it is remarkable to suppress effect, does not have the not enough problems of protection such as relevant container to device, does not have the problem of blocking pipe.Identical with oil soluble from the agent structure of inhibitor, be tetrahydroglyoxaline series all, inhibitor provided by the invention is water miscible from chemical property.Therefore, film-forming properties, the temperature tolerance of the existing oil soluble inhibitor of inhibitor of the present invention, be difficult for the characteristics such as variation of emulsification, anti-pH value, water-soluble inhibitor good solubility, dispersiveness are arranged again, easy to use.Under laboratory condition, do corrosive medium with saturated hydrogen sulfide solution, with the inhibitor of rotary hanging plate weight-loss method evaluation with method for preparing, consumption is when 20mg/L, and inhibiting rate is more than 90%, and consumption is when 50mg/L, and inhibiting rate is more than 95%.
Embodiment
Describe the present invention in detail with specific embodiment below, but embodiment does not limit the scope of the invention.
Example 1:I) preparation inhibiter:
170 gram oleic acid, 90 gram triethylene tetramines, 50 gram dimethylbenzene are added in the four neck flasks simultaneously, are furnished with thermometer, condenser, water trap, agitator and heating unit.Be heated to 150 ℃ and begin distillation, constant temperature was warmed up to 200 ℃ with 10 ℃/h after 3 hours, and constant temperature 5 hours makes binary system be condensed into the oil-soluble intermediate that contains the bicyclic imidazo quinoline; Get 100 gram intermediates, add 40 gram ethanol, under agitation condition, slowly add 20 gram vinylformic acid, add the back and continue to stir 1 hour, make it to be converted into inhibiter.
II) preparation inhibitor
With step I) in the preparation inhibiter and zinc sulfate composite at normal temperatures and pressures, wherein inhibiter accounts for 95 weight %, agent is inhibited.
Example 2: 1 preparation method is identical with example, and just changing oleic acid into molecular-weight average is about 260 naphthenic acid.
Example 3: 1 preparation method is identical with example, just changes oleic acid into linolic acid, triethylene tetramine changes tetraethylene pentamine into.
Example 4: 1 preparation method is identical with example, just 170 gram oleic acid is changed into 100 gram linolic acid and the stearic mixture of 100 grams, and 90 gram triethylene tetramines change the mixture of 40 gram triethylene tetramines and 50 tetraethylene pentamine into.
Example 5: 1 preparation method is identical with example, just 170 gram oleic acid, 90 gram triethylene tetramines is changed into 130 gram molecular-weight average and is about 260 naphthenic acid, 95 gram tetraethylene pentamine.
Example 6: 1 preparation method is identical with example, just changes 170 gram oleic acid, 90 gram triethylene tetramines into 130 gram oleic acid, 140 gram triethylene tetramines.
Example 7: 1 preparation method is identical with example, just 50 gram dimethylbenzene is changed into the mixture of 35 gram toluene and 35 gram dimethylbenzene.
Example 8: 1 preparation method is identical with example, just changes zinc sulfate into zinc acetate, and ethanol changes butanols into, and vinylformic acid changes acetate into.
Example 9: 1 preparation method is identical with example, just will be warmed up to 200 ℃ with 10 ℃/h, and constant temperature 5 hours makes to be warmed up to 220 ℃ with 10 ℃/h constant temperature 3 hours into.
Example 10: 1 preparation method is identical with example, just will be warmed up to 200 ℃ with 10 ℃/h, and constant temperature 5 hours makes to be warmed up to 240 ℃ with 10 ℃/h constant temperature 10 hours into.
Example 11: 1 preparation method is identical with example, just changes 40 gram ethanol into 60 gram butanols.
Example 12: 1 preparation method is identical with example, and just inhibiter is accounted for 95 weight % accounts for 90 weight % instead.
Example 13: 9 preparation methods are identical with example, just change 40 gram ethanol into 80 gram ethanol.
Example 14: 10 preparation methods are identical with example, and just inhibiter is accounted for 95 weight % accounts for 90 weight % instead.
Example 15: 13 preparation methods are identical with example, just change zinc sulfate into Zinc Gluconate, and vinylformic acid changes acetate into, and inhibiter accounts for 95 weight % and accounts for 90 weight % instead.
Example 16: laboratory condition is estimated with reference to the rotary hanging plate method in " water coolant analysis and test method " down.Corrosive medium is the saturated aqueous solution of hydrogen sulfide, inhibitor respectively by 0,10,20,50mg/L concentration joins in the corrosive medium, the A3 steel of selecting 25*10*2mm for use is as test piece, be dipped in the corrosive medium, speed of rotation is 75 rev/mins, and experimental period is 6 hours, and experimental temperature is 40 ± 1 ℃.Each concentration test has three parallel test pieces, calculates average corrosion rate (mm/a), i.e. corrosion rate.Be calculated as follows:
F = C · ΔW A · T · ρ
In the formula: the C-computational constant, when being unit with mm/a, C=8.76 * 10 7,
The corrosion weight loss (g) of Δ w-test specimen,
Area (the cm of A-test specimen 2),
The T-corrosion test time (h);
Density (the kg/m of ρ-material for test 3).
Corrosion inhibition rate is calculated as follows:
Fo corrosion rate when not adding inhibiter (blank);
Fk is the corrosion rate when adding inhibiter.
Test-results sees Table 1.
Table 1 inhibitor test evaluation data
Test conditions: hydrogen sulfide saturated aqueous solution; Soak rotation; 6 hours; 40 ± 1 ℃
Numbering The inhibiter kind Concentration mg/L Average weightless mg Corrosion rate mm/a Corrosion inhibition rate %
??1 Blank ??0 ??11.4 ??3.33
??2 Example 1 product ??10 ??2 ??0.585 ??82.4
??3 Example 1 product ??20 ??0.7 ??0.205 ??93.8
??4 Example 1 product ??50 ??0.3 ??0.088 ??97.4
??5 Example 2 products ??10 ??2.3 ??0.673 ??79.8
??6 Example 3 products ??20 ??1 ??0.292 ??91.2
??7 Example 4 products ??50 ??0.4 ??0.117 ??96.5
??8 Example 5 products ??10 ??2.5 ??0.731 ??78.0
??9 Example 6 products ??20 ??0.5 ??0.263 ??95.6
??10 Example 7 products ??50 ??0.3 ??0.088 ??97.4
??11 Example 8 products ??10 ??2 ??0.585 ??82.4
??12 Example 9 products ??20 ??0.5 ??0.263 ??95.6
??13 Example 10 products ??50 ??0.4 ??0.117 ??96.5
??14 Example 11 products ??10 ??1.8 ??0.526 ??84.2
??15 Example 12 products ??20 ??0.8 ??0.234 ??93.0
??16 Example 13 products ??50 ??0.2 ??0.059 ??98.2
??17 Example 14 products ??10 ??1.9 ??0.556 ??83.3
??18 Example 15 products ??20 ??0.9 ??0.263 ??92.1

Claims (10)

1. inhibitor, it is characterized in that: this inhibitor is made up of the inhibiter of 90-97 weight % and the protection against corrosion promotor of 3-10 weight %, and wherein the general structure of inhibiter is as the formula (1):
R is alkyl or alkylene, cycloalkyl group or the cycloalkenyl group that the straight chain of 8～30 carbon atoms is arranged or have side chain in the formula, and the structural formula of R ' is
Figure A2004100103180002C2
, wherein n1 is 0～4 integer: protection against corrosion promotor is organic acid zinc salt or mineral acid zinc salt.
2. inhibitor according to claim 1 is characterized in that: the carbonatoms of described R is 12～24.
3. inhibitor according to claim 1 is characterized in that: described protection against corrosion promotor is zinc sulfate, zinc nitrate, zinc acetate or Zinc Gluconate.
4. one kind prepares the method for inhibitor according to claim 1, it is characterized in that this method comprises the steps:
I) preparation inhibiter
(a) organic acid and polyethylene polyamine are 1～5: 5～1 mixing in molar ratio, 5～30% the azeotropic agent that adds reactant weight then, be warmed up to 140-160 ℃, constant temperature 1～10 hour, be warmed up to 200～240 ℃ with 10 ℃ speed per hour then, constant temperature 3～10 hours makes binary system be condensed into the oil-soluble intermediate that contains the bicyclic imidazo quinoline:
Wherein said organic acid is aliphatic carboxylic acid, alicyclic carboxylic acid or their mixture;
Aliphatic carboxylic acid is the straight chain of 8～30 carbon atoms to be arranged or have side chain, saturated or undersaturated carboxylic acid;
Alicyclic carboxylic acid is that molecular-weight average is 240～500, has the carboxylic acid of 1～5 ring;
Azeotropic agent is an aromatic hydrocarbon solvent;
The structural formula of polyethylene polyamine is H 2N (CH 2CH 2NH) N2CH 2CH 2NH 2, wherein n2 is 2～6 integer;
(b) add solubility promoter in step (a) gained intermediate, under agitation condition, slowly add transforming agent, whole dropping and reaction times are 1～3 hour, make it to be converted into inhibiter;
Wherein said solubility promoter is the Fatty Alcohol(C12-C14 and C12-C18) that 2～4 carbon atoms are arranged, and usage quantity is 20～100% of an intermediate weight;
Transforming agent is the aliphatic carboxylic acid that 1～4 carbon atom is arranged, and usage quantity is 20～50% of an intermediate weight, also can determine usage quantity according to the system pH value, when the pH value of whole system 7～8 the time, can stop to drip;
II) preparation inhibitor
The inhibiter and the protection against corrosion promotor of preparation in the step (I) is composite at normal temperatures and pressures, obtain inhibitor of the present invention.
5. preparation method according to claim 4 is characterized in that: the carbonatoms in the aliphatic carboxylic acid is 12～24; The molecular-weight average of alicyclic carboxylic acid is 260～300.
6. according to claim 4 or 5 described preparation methods, it is characterized in that: the carbon number of the ring in the alicyclic carboxylic acid is 5 or 6.
7. preparation method according to claim 4 is characterized in that: aliphatic carboxylic acid is monobasic or binary lipid acid; Naphthenic acid is the monobasic naphthenic acid.
8. preparation method according to claim 7 is characterized in that: aliphatic carboxylic acid is oleic acid, linolic acid, stearic acid or dodecenylsuccinic acid.
9. preparation method according to claim 4 is characterized in that: azeotropic agent is the mononuclear aromatics solvent; Polyethylene polyamine is triethylene tetramine, tetraethylene pentamine, five ethene hexamines or their mixture; Solubility promoter is ethanol, propyl alcohol, Virahol or butanols; Transforming agent is formic acid, acetate or vinylformic acid.
10. the application of the described inhibitor of claim 1 is characterized in that: this inhibitor is used to contain H 2S-H 2The O system joins inhibitor of the present invention during use and contains H with the consumption of 5～150mg/L 2S-H 2In the system of O.
CN 200410010318 2004-06-04 2004-06-04 Inhibitor, preparing method and use thereof Expired - Fee Related CN1283838C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105874101A (en) * 2013-12-27 2016-08-17 陶氏环球技术有限责任公司 Corrosion inhibiting compositions including bis-imidazoline compounds derived from enriched linear tetramines
CN108440415A (en) * 2018-05-17 2018-08-24 洛阳理工学院 A kind of oil-soluble bi-imidazoline derivative corrosion inhibiter and its preparation method and application
US10428454B2 (en) 2013-12-27 2019-10-01 Dow Global Technologies Llc Textile treatment compositions including quternary bis-imidazoline compounds derived from linear tetramines useful to improve moisture management and provide antimicrobial protection
US10487406B2 (en) 2013-12-27 2019-11-26 Dow Global Technologies Llc Bis-imidazoline compounds as corrosion inhibitors and preparation thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105874101A (en) * 2013-12-27 2016-08-17 陶氏环球技术有限责任公司 Corrosion inhibiting compositions including bis-imidazoline compounds derived from enriched linear tetramines
US10329672B2 (en) 2013-12-27 2019-06-25 Dow Global Technologies Llc Corrosion inhibiting compositions including bis-imidazoline compounds derived from enriched linear tetramines
US10428454B2 (en) 2013-12-27 2019-10-01 Dow Global Technologies Llc Textile treatment compositions including quternary bis-imidazoline compounds derived from linear tetramines useful to improve moisture management and provide antimicrobial protection
US10487406B2 (en) 2013-12-27 2019-11-26 Dow Global Technologies Llc Bis-imidazoline compounds as corrosion inhibitors and preparation thereof
CN108440415A (en) * 2018-05-17 2018-08-24 洛阳理工学院 A kind of oil-soluble bi-imidazoline derivative corrosion inhibiter and its preparation method and application
CN108440415B (en) * 2018-05-17 2020-11-06 洛阳理工学院 Oil-soluble bis-imidazoline derivative corrosion inhibitor and preparation method and application thereof

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