CN104562035B - Silicon-containing corrosion inhibitor composition and preparation method thereof - Google Patents
Silicon-containing corrosion inhibitor composition and preparation method thereof Download PDFInfo
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Abstract
The invention provides a silicon-containing corrosion inhibitor composition and a preparation method thereof. The silicon-containing corrosion inhibitor composition comprises methyl phenyl hydrogen-containing polysiloxane, 2-mercaptobenzothiazole, benzothiazolol, a chloroplatinic acid isopropanol solution, a phosphite ester compound, a solvent A and a solvent B. The preparation method of the silicon-containing corrosion inhibitor composition comprises the following steps: adding methyl phenyl hydrogen-containing polysiloxane, 2-mercaptobenzothiazole and benzothiazolol into the solvent A, dropwise adding the chloroplatinic acid isopropanol solution at 70-80 DEG C, performing reaction for 4-10 h in the presence of nitrogen, and removing the solvent from a reaction mixture to obtain a primary product M; and adding the primary product M into the solvent B, then adding the phosphite ester compound, and stirring for 1-5 h at 50-80 DEG C to obtain the silicon-containing corrosion inhibitor composition. The silicon-containing corrosion inhibitor composition provided by the invention has better heat stability, better environmental suitability and a stronger adsorption film forming characteristic, and is low in usage amount and high in continuous corrosion resistance.
Description
Technical field
The present invention relates to a kind of composite corrosion inhibitor and its synthetic method, more particularly to one kind can significantly reduce metal tube
Road inner wall corrosion speed, effectively improves siliceous composite corrosion inhibitor of device corrosion resistance and preparation method thereof, belongs to corrosion anti-
Protector for collar domain.
Background technology
Crude oil gradually heaviness and in poor quality in recent years, and oil product constantly requires lighting and cleans, and increases
Add crude oil difficulty of processing, the etching problem in production process also seems and is particularly acute, the corruption producing particularly in oil refining process
Corrosion material brings serious threat to safety in production.Various countries always all attach great importance to etching problem.
Corrosion inhibiter is a kind of anticorrosion chemicals, is to be present in environment (medium) with debita spissitudo and form, can in case
Stop or slow down a kind of chemical substance of corrosion generation or the mixture of several chemical substance.Since half a century, the product of corrosion inhibiter
Plant and constantly update, quality improves constantly, and serves irreplaceable effect, inhibition in terms of slowing down the burn into extension device life-span
Agent has become one of important anti-corrosion measure.
Corrosion inhibiter has the features such as high selectivity, leachability, contaminative, toxic, the protective capability of equipment is subject to various
Factor affects, such as the chemical composition of corrosion inhibiter and property, implantation concentration and operative temperature, environment pH value, corrosive medium institute
In system flow velocity etc., in addition also relevant with device structure, injection position etc..
At present, the absorption film-forming type corrosion inhibiter that oil plant is commonly used mainly has pyridines, amide-type and imidazoline corrosion inhibitor,
Their common feature is to contain nitrogen-atoms in molecule, and its corrosion inhibition mainly leans on nitrogen-atoms and the suction-operated of metal to come in fact
Existing.But the restriction due to synthetic technology, the quality of product is uneven, also unstable.In addition, the imidazoline of long alkyl side chain
Or amide-type corrosion inhibiter has hydrolysis temperature relatively low, structural instability at relatively high temperatures, continue corrosion resistance not strong, to some tools
The features such as device having complex internal structure adapts to poor, is therefore susceptible to lose efficacy under some special occasions or causes corruption
The problems such as erosion aggravation.
Content of the invention
Weak for the corrosion inhibiter thermal adaptability such as alkyl imidazoline in prior art and amide-type, some gold at high temperature
Belong to the defects such as inner member surface filming is unstable, the invention provides a kind of there is good heat stability, outstanding surface becomes
Membrane property and the stable siliceous composite corrosion inhibitor of anti-corrosion film Rotating fields and preparation method thereof.
Siliceous composite corrosion inhibitor of the present invention, including following component：Aminomethyl phenyl hydrogen containing siloxane, 2- sulfydryl benzene
And thiazole, hydroxybenzothiazole, isopropyl alcohol solution of chloroplatinic acid, phosphite ester compound, solvent orange 2 A and solvent B.
In the siliceous composite corrosion inhibitor of the present invention, described aminomethyl phenyl hydrogen containing siloxane, molecular weight 1000 ~ 10000, excellent
Molecular weight is selected to be 1000 ~ 5000, most preferably molecular weight is 1500 ~ 3500, active hydrogen content is 0.2wt% ~ 2.0wt%, preferably alive
Property hydrogen content 0.2wt % ~ 1.0wt%, most preferably active hydrogen content 0.3wt % ~ 0.5wt%, with the molar fraction on main chain, benzene
Base content is 1% ~ 5%, preferably phenyl content 1% ~ 2.5%, most preferably phenyl content 1.5% ~ 2.5%.Described aminomethyl phenyl is hydrogeneous poly-
Addition in prepared by siliceous composite corrosion inhibitor for the siloxanes is 5 ~ 25 mass parts, preferably 5 ~ 15 mass parts, most preferably 5 ~ 10
Mass parts.
In the siliceous composite corrosion inhibitor of the present invention, described 2-mercaptobenzothiazole is in prepared by siliceous composite corrosion inhibitor
Addition is 0.1 ~ 2 mass parts, preferably 0.25 ~ 1.0 mass parts, most preferably 0.5 ~ 0.75 mass parts.
In the siliceous composite corrosion inhibitor of the present invention, described hydroxybenzothiazole is in prepared by described siliceous composite corrosion inhibitor
Addition be 0.1 ~ 3 mass parts, preferably 0.5 ~ 2.0 mass parts, most preferably 0.8 ~ 1.0 mass parts.
In the siliceous composite corrosion inhibitor of the present invention, described phosphite ester compound be selected from diisooctyl phenyl phosphite,
One of triphenyl phosphite, phosphorous acid three monooctyl ester or two or more mixtures, preferably diisooctyl phenyl phosphite, Asia
Trioctyl phosphate, addition in prepared by siliceous composite corrosion inhibitor for the phosphite ester compound is 1 ~ 20 mass parts, preferably 5
~ 15 mass parts, most preferably 8 ~ 12 mass parts.
In siliceous composite corrosion inhibitor of the present invention, described solvent orange 2 A is normal heptane, isoheptane, arbitrary in isooctane
Kind, preferably normal heptane；Addition in prepared by siliceous composite corrosion inhibitor for the solvent orange 2 A is 100 ~ 500 mass parts, preferably 100 ~
350 mass parts, most preferably 150 ~ 250 mass parts.
In the siliceous composite corrosion inhibitor of the present invention, described solvent B is toluene, normal octane, dimethylbenzene, n-octyl alcohol, isooctanol
In any one, preferably toluene；Addition in prepared by siliceous composite corrosion inhibitor for the solvent B is 100 ~ 500 mass parts, preferably
100 ~ 350 mass parts, most preferably 150 ~ 250 mass parts.
In the siliceous composite corrosion inhibitor of the present invention, in catalyst isopropyl alcohol solution of chloroplatinic acid, Pt content is 0.1 ~ 1.5wt%,
Preferably 0.1 ~ 0.5wt%；Addition in prepared by described siliceous composite corrosion inhibitor for the described isopropyl alcohol solution of chloroplatinic acid catalyst
For 0.01 ~ 0.1 mass parts, preferably 0.025 ~ 0.075 mass parts, most preferably 0.05 ~ 0.075 mass parts.
The present invention siliceous composite corrosion inhibitor preparation method is as follows：
（1）Under agitation, aminomethyl phenyl hydrogen containing siloxane, 2-mercaptobenzothiazole and hydroxybenzothiazole are added
Enter in solvent orange 2 A, then heat up, drip isopropyl alcohol solution of chloroplatinic acid when 70 ~ 80 DEG C, reaction 4 ~ 10 is little under nitrogen protection
When, after reactant mixture removes solvent, obtain a product M it is ensured that residual activity hydrogen content is less than 0.05wt% in product M；
（2）Product M is added in solvent B, is subsequently adding phosphite ester compound, at 50 ~ 80 DEG C, stir 1 ~ 5
Hour, obtain final product described siliceous composite corrosion inhibitor.
In the inventive method, can be remaining by IR quantitative analysis or product M of nuclear magnetic resonance internal mark method determination
Active hydrogen content, if residual activity hydrogen content ＞ 0.05wt%, repeat step in M（1）, continue reaction 2 hours or more, until
Residual activity hydrogen content is down to below 0.05wt %.
When using, can be used according to device needs by a certain percentage by corrosion inhibiter the siliceous composite corrosion inhibitor of the present invention
Composition is dispersed in ethanol, acetone, gasoline, diesel oil and kerosene equal solvent and uses.
Compared with prior art, advantages of the present invention is as follows：
By siliceous composite corrosion inhibitor of the present invention, its active component is to be in aminomethyl phenyl hydrogen containing siloxane
On the linear macromolecule of main chain, scion grafting has multiple substituted radicals of adsorption activity, this knot on the metal inner surface surface of device
Structure makes to have carried multiple active adsorption sites on each linear macromolecule, therefore than alkyl imidazoline of the prior art or alkyl
Amide-type corrosion inhibiter has higher adsorption activity, and " pinning " effect that many avtive spots adsorb in metal surface simultaneously simultaneously is big
Improve greatly the stability of corrosion inhibiter bioactive molecule absorption film-forming, in addition the presence of the phenyl substituent on siloxane main chain is not only
Enhance the heat endurance of molecule, its stronger electron characteristic also contributes to improve the electron energy of the nitrogenous substituent closing on
Power, makes absorption affinity higher.
Local invent described high-temperature corrosion inhibitor it does not only have the change more more stable than alkyl chain as the polysiloxanes of main chain
Learn structure and more stable chemical property, also have very strong compliance simultaneously, therefore its molecule is permissible when adsorbing in metal surface
According to reduce sterically hindered need by the bending of arbitrarily angled or direction, rotate, this characteristic is more conducive to multiple on main chain
The absorption film-forming at high proportion of substituent.
Polymethyl siloxane free end after the absorption of metal surface for the siliceous corrosion inhibiter of the present invention, has more common
Metal surface therefore can be intercepted by long alkyl side chain higher hydrophobicity effectively with the Korrosionsmedium such as condensation, recirculation water
Come, substantially reduce the corrosion rate in device；In addition, the polymethyl siloxane free end after above-mentioned absorption carries some activity
Group, can occur self-crosslinking reaction at certain temperature and ambient condition, and then forms one in metal surface to a certain extent
Layer " absorption self-crosslinking film ", can preferably protect hardware from dielectric corrosion.
In siliceous corrosion inhibiter of the present invention, the wherein molecule of siloxane polymer containing thiazole contain multiple can be with metal watch
The thiazole structure of face absorption, can make inhibitor molecular be firmly adsorbed on metal surface, overcome adsorbed film appearance caducous
Shortcoming, the film that phosphite ester is formed simultaneously belongs to precipitation membrane, can adsorb the gap in nitrogenous sulfur-bearing polymer adsorbed film, make
Overall adsorbed film is finer and close, thus substantially increasing the slow release effect of corrosion inhibiter.
It is good that siliceous corrosion inhibiter of the present invention also has a solvent compatibility, applied widely, both can mix in the feed
Enter it is also possible in the dilution filling of crucial protection position, consumption can be adjusted flexibly according to working condition, have longer lasting resistance to
Abrasion cycle, low toxicity, advantages of environment protection, are a kind of new and effective broad spectrum type metal surface corrosion inhibition agent.
With reference to specific embodiment, the present invention is further elaborated.
Specific embodiment
With reference to specific embodiment, the present invention is described further, but the present invention is not limited to these enforcements
Example.
Embodiment 1
Average molecular weight of making even is 2000 aminomethyl phenyl hydrogen containing siloxane（Active hydrogen content is 0.5wt%, phenyl content
1.5~2.5wt%）10g, 2-mercaptobenzothiazole 0.7g and hydroxybenzothiazole 0.4g, add the round bottom equipped with 350mL normal heptane
In flask, successively stirring is warming up to 75 ± 5 DEG C in water bath with thermostatic control simultaneously, then adds about 10 0.05mol/ with dropper
L isopropyl alcohol solution of chloroplatinic acid, course of reaction is carried out 5 hours under nitrogen protection, and reactant mixture is carried out vacuum distillation removal
Solvent n-heptane, that is, obtain siloxane polymer containing thiazole.By residual activity in nuclear magnetic resonance internal mark method determination purpose product
Hydrogen content is about 0.01%wt., and product is qualified.Then upper step is obtained product to add in 400mL toluene, is subsequently adding phosphorous
A sour benzene di-isooctyl, at 70 DEG C, stirs 4 hours, obtains final product the high-temperature corrosion inhibitor of present invention offer.Take hydrofinishing kerosene conduct
Solvent, synthetic product is made into 1% kerosin.
Embodiment 2
Average molecular weight of making even is 2000 aminomethyl phenyl hydrogen containing siloxane（Active hydrogen content is 0.3wt%, phenyl content 2
~2.5wt%）10g, 2-mercaptobenzothiazole 0.7g and hydroxybenzothiazole 0.4g, add the round bottom equipped with 350mL normal heptane to burn
In bottle, successively stirring is warming up to 75 ± 5 DEG C in water bath with thermostatic control simultaneously, then adds about 15 0.05mol/L with dropper
Isopropyl alcohol solution of chloroplatinic acid, course of reaction is carried out 6 hours under nitrogen protection, reactant mixture is carried out vacuum distillation removal molten
Agent normal heptane, that is, obtain siloxane polymer containing thiazole.By residual activity hydrogen in nuclear magnetic resonance internal mark method determination purpose product
Content is about 0.01%wt., and product is qualified.Then upper step is obtained product to add in 350mL toluene, is subsequently adding phosphorous acid
Three monooctyl esters, at 70 DEG C, stir 4 hours, obtain final product the high-temperature corrosion inhibitor of present invention offer.Take hydrofinishing kerosene as solvent, will
Synthetic product is made into 1% kerosin.
Embodiment 3
Average molecular weight of making even is 1500 aminomethyl phenyl hydrogen containing siloxane（Active hydrogen content is 0.5wt%, phenyl content
1.5~2.5wt%）10g, 2-mercaptobenzothiazole 0.75g and hydroxybenzothiazole 0.5g, add the circle equipped with 350mL normal heptane
In the flask of bottom, successively stirring is warming up to 70 ± 5 DEG C in water bath with thermostatic control simultaneously, then adds about 10 with dropper
0.05mol/L isopropyl alcohol solution of chloroplatinic acid, course of reaction is carried out 5 hours under nitrogen protection, and reactant mixture is reduced pressure
Distillation removes solvent n-heptane, that is, obtain siloxane polymer containing thiazole.By in nuclear magnetic resonance internal mark method determination purpose product
Residual activity hydrogen content is about 0.01%wt., and product is qualified.Then upper step is obtained product and adds in 400mL toluene, then
Add diisooctyl phenyl phosphite, at 60 DEG C, stir 3 hours, the high-temperature corrosion inhibitor of present invention offer is provided.Take hydrofinishing
Diesel oil, as solvent, synthetic product is made into 1% diesel oil solution.
Embodiment 4
Average molecular weight of making even is 2500 aminomethyl phenyl hydrogen containing siloxane（Active hydrogen content is 0.5wt%, phenyl content
1.5~2.5wt%）10g, 2-mercaptobenzothiazole 0.7g and hydroxybenzothiazole 0.4g, add the round bottom equipped with 350mL isooctane
In flask, successively stirring is warming up to 75 ± 5 DEG C in water bath with thermostatic control simultaneously, then adds about 10 0.05mol/ with dropper
L isopropyl alcohol solution of chloroplatinic acid, course of reaction is carried out 5 hours under nitrogen protection, and reactant mixture is carried out vacuum distillation removal
Solvent n-heptane, that is, obtain siloxane polymer containing thiazole.By residual activity in nuclear magnetic resonance internal mark method determination purpose product
Hydrogen content is about 0.01%wt., and product is qualified.Then upper step is obtained product to add in 400mL toluene, is subsequently adding phosphorous
A sour benzene di-isooctyl, at 65 DEG C, stirs 4 hours, obtains final product the high-temperature corrosion inhibitor of present invention offer.Take hydrofining diesel oil conduct
Solvent, synthetic product is made into 1% diesel oil solution.
Certain commercially available imidazolines oil-soluble inhibitor chosen by corrosion inhibiter in comparative example, by the respective concentration in embodiment
Prepare the diesel oil solution of corresponding ratio.
Composite corrosion inhibitor performance test：
According to ASTM G170-06 " Standard Guide for Evaluating and Qualifying
Oilfield and Refinery Corrosion Inhibitors in the Laboratory " standard specifies, carries out mould
Intend the dynamically weightless coupon test test under working condition.Test condition is as follows：55 ± 5 DEG C of test temperature, test period 72h,
Rotating speed 0.5m/s, lacing film material L360 carbon steel（50mm×20mm×2mm）.
Volume for 4L high-potting kettle in add 2.5L crude distillation simulated solution, and 1% above-mentioned corrosion inhibiter bavin
Oil solution 0.02g, after relaxing uniformly, is filled with a certain amount of N into kettle2, after sealing, carry out experiment test（Carry out one group of blank simultaneously
Contrast experiment）.
Test result：Blank assay lacing film average corrosion rate is about 0.88mm/a, and corrosion inhibition rate is calculated as follows：Slow
Erosion rate=[（The actual rate of corrosion of blank assay rate of corrosion）/ blank assay rate of corrosion] × 100%
The corrosion inhibition contrast of the various organosilicon composite corrosion inhibitor of table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example | |
| Corrosion rate, mm/a | 0.070 | 0.069 | 0.045 | 0.068 | 0.137 |
| Corrosion inhibition rate, % | 93.26 | 93.18 | 94.51 | 91.31 | 82.04 |
Claims (13)
1. a kind of siliceous composite corrosion inhibitor is it is characterised in that described composite corrosion inhibitor raw material includes：5 ~ 25 mass parts methyl
Phenyl hydrogen containing siloxane, 0.1 ~ 2 mass parts 2-mercaptobenzothiazole, 0.1 ~ 3 mass parts hydroxybenzothiazole, 0.01 ~ 0.1 matter
Amount part isopropyl alcohol solution of chloroplatinic acid, 1 ~ 20 mass parts phosphite ester compound, 100 ~ 500 mass parts solvent orange 2 As and 100 ~ 500 matter
Amount part solvent B, described solvent orange 2 A is normal heptane, isoheptane, any one in isooctane, described solvent B is toluene, normal octane, two
Any one in toluene, n-octyl alcohol, isooctanol.
2. siliceous composite corrosion inhibitor according to claim 1 it is characterised in that：Described composite corrosion inhibitor raw material includes
5 ~ 15 mass parts aminomethyl phenyl hydrogen containing siloxanes, 0.25 ~ 1.0 mass parts 2-mercaptobenzothiazole, 0.5 ~ 2.0 mass parts hydroxyl
Benzothiazole, 0.025 ~ 0.075 mass parts isopropyl alcohol solution of chloroplatinic acid, 5 ~ 15 mass parts phosphite ester compounds, 100 ~ 350
Mass parts solvent orange 2 A and 100 ~ 350 mass parts solvent B, described solvent orange 2 A is normal heptane, isoheptane, any one in isooctane, institute
State solvent B be toluene, normal octane, dimethylbenzene, n-octyl alcohol, any one in isooctanol.
3. siliceous composite corrosion inhibitor according to claim 1 it is characterised in that：Described composite corrosion inhibitor raw material includes
5 ~ 10 mass parts aminomethyl phenyl hydrogen containing siloxanes, 0.5 ~ 0.75 mass parts 2-mercaptobenzothiazole, 0.8 ~ 1.0 mass parts hydroxyl
Benzothiazole, 0.05 ~ 0.075 mass parts isopropyl alcohol solution of chloroplatinic acid, 8 ~ 12 mass parts phosphite ester compounds, 150 ~ 250
Mass parts solvent orange 2 A and 150 ~ 250 mass parts solvent B, described solvent orange 2 A is normal heptane, isoheptane, any one in isooctane, institute
State solvent B be toluene, normal octane, dimethylbenzene, n-octyl alcohol, any one in isooctanol.
4. siliceous composite corrosion inhibitor according to claim 1 it is characterised in that：The hydrogeneous poly- silica of described aminomethyl phenyl
Alkane, molecular weight 1000 ~ 10000, active hydrogen content is 0.2wt% ~ 2.0wt%, with the molar fraction phenyl content on main chain is
1%~5%.
5. siliceous composite corrosion inhibitor according to claim 1 it is characterised in that：The hydrogeneous poly- silica of described aminomethyl phenyl
Alkane, molecular weight is 1000 ~ 5000, and active hydrogen content is 0.2wt % ~ 1.0wt%, with the molar fraction phenyl content on main chain
For 1% ~ 2.5%.
6. siliceous composite corrosion inhibitor according to claim 1 it is characterised in that：The hydrogeneous poly- silica of described aminomethyl phenyl
Alkane, molecular weight is 1500 ~ 3500, and active hydrogen content is 0.3wt % ~ 0.5wt%, with the molar fraction phenyl content on main chain
For 1.5% ~ 2.5%.
7. siliceous composite corrosion inhibitor according to claim 1 it is characterised in that：Described phosphite ester compound is selected from
One of diisooctyl phenyl phosphite, triphenyl phosphite, phosphorous acid three monooctyl ester or two or more mixtures.
8. siliceous composite corrosion inhibitor according to claim 1 it is characterised in that：Described phosphite ester compound phosphorous
A sour benzene di-isooctyl, phosphorous acid three monooctyl ester.
9. siliceous composite corrosion inhibitor according to claim 1 it is characterised in that：Described solvent orange 2 A is normal heptane.
10. siliceous composite corrosion inhibitor according to claim 1 it is characterised in that：Described solvent B is toluene.
11. siliceous composite corrosion inhibitors according to claim 1 it is characterised in that：In isopropyl alcohol solution of chloroplatinic acid, Pt contains
Measure as 0.1 ~ 1.5wt%.
12. siliceous composite corrosion inhibitors according to claim 11 it is characterised in that：In isopropyl alcohol solution of chloroplatinic acid, Pt contains
Measure as 0.1 ~ 0.5wt%.
Described in any claim in 13. claims 1 ~ 12, organosilicon composite corrosion inhibitor preparation method, comprises the steps：
(1) under agitation, aminomethyl phenyl hydrogen containing siloxane, 2-mercaptobenzothiazole and hydroxybenzothiazole are added to
In solvent orange 2 A, then heat up, drip isopropyl alcohol solution of chloroplatinic acid when 70 ~ 80 DEG C, under nitrogen protection reaction 4 ~ 10 hours, instead
After answering mixture to remove solvent, obtain a product M it is ensured that residual activity hydrogen content is less than 0.05wt% in product M；
(2) a product M is added in solvent B, is subsequently adding phosphite ester compound, at 50 ~ 80 DEG C, stir 1 ~ 5 hour,
Obtain final product described siliceous composite corrosion inhibitor.
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| CN1387961A (en) * | 2002-05-20 | 2003-01-01 | 东南大学 | Composite self-assembling method of organic superthin corrosion inhibiting film |
| WO2008009680A1 (en) * | 2006-07-17 | 2008-01-24 | Technische Universität Bergakademie Freiberg | Novel hydrogen-rich 1,3-dialkoxydisiloxanes and processes for their preparation and their use |
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| CN1387961A (en) * | 2002-05-20 | 2003-01-01 | 东南大学 | Composite self-assembling method of organic superthin corrosion inhibiting film |
| WO2008009680A1 (en) * | 2006-07-17 | 2008-01-24 | Technische Universität Bergakademie Freiberg | Novel hydrogen-rich 1,3-dialkoxydisiloxanes and processes for their preparation and their use |
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