CN103225081B - Corrosion inhibitor used in carbon steel corrosion in ammonia-method desulphurization ammonium sulfate preparation system - Google Patents
Corrosion inhibitor used in carbon steel corrosion in ammonia-method desulphurization ammonium sulfate preparation system Download PDFInfo
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- CN103225081B CN103225081B CN201310150090.8A CN201310150090A CN103225081B CN 103225081 B CN103225081 B CN 103225081B CN 201310150090 A CN201310150090 A CN 201310150090A CN 103225081 B CN103225081 B CN 103225081B
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Abstract
The invention relates to a corrosion inhibitor used in carbon steel corrosion in an ammonia-method desulphurization ammonium sulfate preparation system. The corrosion inhibitor is composed of, by weight, 20-80% of a thiourea derivative, 10-50% of organic amine, and 5-40% of imidazoline quaternary ammonium salt. The thiourea derivative is one selected from phenyl thiourea, diphenyl thiourea, thiosemicarbazide and propenyl thiourea. The organic amine is one selected from polyacrylamide, dodecylamine, hexadecylamine and octadecylamine. The chemical structural formula of the imidazoline quaternary ammonium salt is shown in the description, wherein R is phenyl, C2-C11 straight-chain alkyl, CH3(CH2)7CH=CH(CH2)7 or CH3(CH2)9CH=CH(CH2)7, and n is 2, 3, or 4. The corrosion inhibitor has good corrosion inhibiting performance. When the corrosion inhibitor is applied in inhibiting the corrosion in the ammonia-method desulphurization ammonium sulfate preparation system, the dose is low, and application is simple and convenient.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of inhibiter being applicable to the corrosion of ammonia process of desulfurization Sulphuric acid ammonium system medium carbon steel.
Technical background
The ammonia process of desulfurization is with certain density ammoniacal liquor for sweetening agent, generates ammonium sulphite, then changes into ammonium sulfate byproduct by atmospheric oxygen, reach the object of flue gas desulfurization with the sulfurous gas removed in flue gas.Therefore, in the solution of desulfurization sulphur ammonium system, sulfate concentration is very high, and can reach a hundreds of thousands of ppm, solution ph is between 4-6 in addition, is slightly acidic, and temperature is at about 40 DEG C, and etching problem is quite serious.Liu Yuesheng etc. systematically analyze the mechanism of corrosion of equipment in ammonia method desulfurizing system and the possible corrosive medium of each corrosion area and corrodible property, point out that System Solution pH is on the low side, under this low pH condition, the ammonium sulfate corrosion of carbon steel is rot-resistant emphasis (" China Power education " 2005, (S2): 1-3).Zhao Wenkai etc. find that corrosion leakage problem appears in equipment, pipeline in ammonium sulfate production, point out stainless corrosion mainly galvanic corrosion, wherein intergranular corrosion and pitting tendency serious (" equipment control and maintenance " 2010, (9): 41-43).
At present, for the etching problem of carbon steel in ammonia process of desulfurization sulphur ammonium system, mainly protect corrosion by adding corrosion protective lining to equipment and applying preservative coat.Lining or the preservative coat material of application mainly contain glass resin flake, isoprene-isobutylene rubber and steel alloy.As protective system, glass resin flake and isoprene-isobutylene rubber have the advantages such as good permeability resistance, higher physical strength and solidity to corrosion, and ammonia-process desulfurization technique is widely used.But its limited solvent resistant ability and resistance to alkali ability make its use be subject to certain restrictions.In addition, glass resin flake is strict to construction requirement.There is pin hole and bulge in the corrosion-resistant coating caused due to construction wrong, and then causes the example (" corrosion and protection " 2010,31 (8): 654-656) of common occurrence of corrosion-resistant coating perforation.Compared with the matrix material of non-metallic liner, nickelalloy has superiority in internal stress, the infiltration of anti-medium and the guarantee of construction quality, but solidity to corrosion is not as rubber and flake paint, and price very expensive (" corrosion and protection " 2005,26 (12): 530-533).In sum, add the method investment cost of protecting protective layer relatively high, strict to construction requirement, the construction technology of impregnating material all has a great impact the life-span of impregnating material and performance etc., and maintenance cycle is between 10 ~ 15 years.
Inhibiter process for protecting is easy, with low cost, practical, occupies an important position in metal protection engineering, plays more and more important effect in the development of the national economy.Fernand Wei Kaman (publication number CN1558940A) disclose a kind of prevent ammonium chloride and ammonium sulfate from causing dirt and the method for corrosion, point out that the corrosion that ammonium chloride produces can be reduced to 1.27 millimeters/year by choline or derivatives thereof, and the generation of dirt can be suppressed completely.
But, be not suitable for the open report of the inhibiter of the corrosion of carbon steel in ammonia process of desulfurization Sulphuric acid ammonium system at present.Therefore; develop a kind of inhibiter of the corrosion of carbon steel be suitable in ammonia process of desulfurization Sulphuric acid ammonium system; think that ammonia process of desulfurization equipment sets up second protection; extend the cycle of shutdown maintenance; be conducive to the widespread use promoting ammonia desulfurizing process, in industry and waste gas pollution control and treatment, there is very important economy and social value.
Summary of the invention
Technical problem to be solved of the present invention is the inhibiter being suitable for the corrosion of ammonia process of desulfurization Sulphuric acid ammonium system medium carbon steel providing a kind of corrosion inhibition high.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
Suppress the inhibiter that carbon steel corrodes in ammonia process of desulfurization Sulphuric acid ammonium system, it is characterized in that, it is made up of thiourea derivative, organic amine and imidazoline quaternary ammonium salt, and wherein the content of each component is by weight percentage: thiourea derivative 20% ~ 80%; Organic amine 10% ~ 50%; Imidazoline quaternary ammonium salt 5% ~ 40%;
Described thiourea derivative is selected from the one in phenylthiourea, diphenyl thiourea, thiosemicarbazide and Allyl thiourea;
Described organic amine is selected from the one in polyacrylamide, amino dodecane, cetylamine and stearylamine;
The chemical structural formula of described imidazoline quaternary ammonium salt is:
Wherein, R is phenyl, C2-C11 straight chained alkyl, CH
3(CH
2)
7cH=CH (CH
2)
7or CH
3(CH
2)
9cH=CH (CH
2)
7; N value is 2,3 or 4.
By such scheme, the content of described each component is preferably by weight percentage: thiourea derivative 65% ~ 75%; Organic amine 15% ~ 25%; Imidazoline quaternary ammonium salt 5% ~ 15%.
By such scheme, described imidazoline quaternary ammonium salt can be commercial commercialization imidazoline quaternary ammonium salt, also can make by oneself by the following method, and concrete preparation method is as follows: by organic carboxyl acid RCOOH, wherein: R is phenyl, C2-C11 straight chained alkyl, CH
3(CH
2)
7cH=CH (CH
2)
7or CH
3(CH
2)
9cH=CH (CH
2)
7, and polyethylene polyamine NH
2cH
2cH
2nH (CH
2cH
2nH)
n-1h, wherein: n value is 2,3 or 4, molar ratio according to 0.5 ~ 1: 1 joins in reaction vessel, by dimethylbenzene: organic carboxyl acid=50 ~ 300: the mol ratio of 1, add dimethylbenzene as azeotropic agent, 130 ~ 170 DEG C of reaction 0.5 ~ 3h, then 180 ~ 240 DEG C are warmed up to, after reaction 2 ~ 3h, cool to 50 DEG C, then dropwise drip Benzyl Chloride wherein while stirring, the mol ratio of described Benzyl Chloride and polyethylene polyamine is 1 ~ 1.5: 1, control temperature is 90 ~ 110 DEG C again, reacts 1 ~ 3h and get final product.
The using method of the inhibiter that above-mentioned suppression carbon steel corrodes in ammonia process of desulfurization Sulphuric acid ammonium system, is characterized in that: it comprises the following steps:
(1) thiourea derivative in inhibiter is mixed with the thiourea derivative aqueous solution;
(2) organic amine in inhibiter is mixed with organic amine ethanolic soln;
(3) imidazoline quaternary ammonium salt in inhibiter is mixed with imidazoline quaternary ammonium salt ethanolic soln;
(4) according to the consumption requirement of inhibiter, and in conjunction with the proportioning of component each in inhibiter, obtain the consumption of each component, then get the solution of each component of respective volume accordingly, join ammonia process of desulfurization Sulphuric acid ammonium system simultaneously, stir.
By such scheme, the mass percent concentration of the described thiourea derivative aqueous solution is 0.5%-5%; The mass percent concentration of described organic amine ethanolic soln is 0.5%-5%; The mass percent concentration of described imidazoline quaternary ammonium salt ethanolic soln is 40%-60%.
By such scheme, the mass percent concentration when inhibiter that described suppression carbon steel corrodes in ammonia process of desulfurization Sulphuric acid ammonium system uses in ammonia process of desulfurization Sulphuric acid ammonium system is 0.05 ~ 0.2%.
The present invention is by selecting thiourea derivative as the main ingredient of this inhibiter; owing to containing two hybridized atom N and hybridized atom S in its molecule; can with the Fe complexing with sky d track; and be adsorbed on steel surface; form insoluble iron sulphide protective membrane; the contact of isolation corrosive medium and carbon steel, plays the object of protection corrosion.Select the specific organic amine and imidazoline quaternary ammonium salt that contain heteroatoms and hydrophobic group as built agent in addition simultaneously, this inhibiter can be improved better in the performance of suppression carbon steel in ammonia process of desulfurization Sulphuric acid ammonium system.
Beneficial effect of the present invention:
Inhibiter corrosion inhibition provided by the invention is good, is applied to consumption when suppressing the corrosion of carbon steel in ammonia process of desulfurization Sulphuric acid ammonium system little, uses simple, convenient.
Accompanying drawing explanation
Fig. 1 is the erosion profile of A3 carbon steel coupon sample in the ammoniumsulphate soln of inhibiter adding different amounts embodiment 1.In figure: the blank ammoniumsulphate soln of a; The add-on 0.05wt% of b inhibiter; The add-on 0.1wt% of c inhibiter; The add-on 0.2wt% of d inhibiter.
Embodiment
Embodiment 1-9
This inhibiter is made up of thiourea derivative, organic amine and imidazoline quaternary ammonium salt, wherein in each embodiment each component choose and content in table 1.
The consumption of component in each embodiment of table 1
Described imidazoline quaternary ammonium salt is
it is by organic carboxyl acid RCOOH and polyethylene polyamine NH
2cH
2cH
2nH (CH
2cH
2nH)
n-1h joins in reaction vessel according to the molar ratio of 1: 1, wherein R and n choose as above table described in, then dimethylbenzene is pressed: organic carboxyl acid=150: the mol ratio of 1, add dimethylbenzene as azeotropic agent, 150 DEG C of reaction 2h, are then warmed up to 200 DEG C, after reaction 2h, cool to 50 DEG C, then dropwise drip Benzyl Chloride wherein while stirring, described Benzyl Chloride and polyethylene polyamine NH
2cH
2cH
2nH (CH
2cH
2nH)
n-1the mol ratio of H is 1: 1, then control temperature is 100 DEG C, reacts 1 ~ 3h and get final product.
The inhibiter of the various embodiments described above is measured its corrosion inhibition by following contrived experiment, specific experiment and result as follows:
(1) thiourea derivative in inhibiter is mixed with the thiourea derivative aqueous solution of 1wt%; Organic amine in inhibiter is mixed with the organic amine ethanolic soln of 1%; Imidazoline quaternary ammonium salt in inhibiter is mixed with the imidazoline quaternary ammonium salt ethanolic soln of 50%; Require (mass percent concentration of inhibiter in system is 0.2%) according to the consumption of inhibiter, and in conjunction with the proportioning (as shown in table 1) of component each in inhibiter, obtain the consumption of each component, then the solution of each component of respective volume is got accordingly, join in 15% ammoniumsulphate soln system simultaneously, and with the ammoniumsulphate soln not adding any inhibiter for blank system, method of polarization curve and weight-loss method is adopted to calculate the corrosion inhibition rate of this inhibiter, specifically respectively in table 2 and table 3 respectively.The single component phenylthiourea of consumption, stearylamine or the imidazoline quaternary ammonium salt such as separately can to add respectively, wherein: R is CH
3(CH
2)
7cH=CH (CH
2)
7n is 2, do ratio, wherein: phenylthiourea, stearylamine, imidazoline quaternary ammonium salt are made into the thiourea derivative aqueous solution of 1wt% respectively in advance, 18 ethanolic solns of 1% and the imidazoline quaternary ammonium salt ethanolic soln of 50%, then according to the add-on of each material, join respectively in 15% ammoniumsulphate soln system, measure its corrosion inhibition.
A. method of polarization curve:
Test materials is with epoxy encapsulation, 1 × 1cm, and surface-area is 1cm
2a3 carbon steel electrode, A3 carbon steel electrode use before, need polish step by step through abrasive paper for metallograph, then through dehydrated alcohol wiping cleaning, cold wind dries up, with drying for standby.
Test mode is as follows: adopt traditional three-electrode system (reference electrode be saturated calomel electrode, supporting electrode be big area platinized platinum), electrochemical test system is tested.Treat the spontaneous potential (E of system
c) stable after, i.e. E in 30min
cfluctuation is no more than scholar 1mV, writes down E
c; Then dynamic potential scanning is started, from E
c-250mV is scanned up to E
c+ 250mV, scanning speed 0.5mV/s, obtain the steady-state polarization of each corresponding system, then try to achieve corresponding corrosion electric current density with this, be calculated as follows corrosion inhibition rate:
In formula: η---corrosion inhibition rate, %;
---the corrosion electric current density under blank condition, A/cm
2;
---add the corrosion electric current density after inhibiter, A/cm
2.
Test result is as follows: compared with blank and reference examples, the steady-state polarization added after isodose the present embodiment 1-9 inhibiter moves to left, and corrosion potential moves to positive dirction, and this shows this inhibiter to control anodic process; Another as can be seen from its corrosion inhibition rate numerical value: after adding embodiment of the present invention inhibiter, the corrosion resistance nature of A3 carbon steel electrode obtains and improves widely.
The parameter fitting result of table 2A3 carbon steel electrode after adding different inhibiter
B. weight-loss method
Test materials: size of sample is 5 × 1 × 0.3cm, surface-area is 13.6cm
2a3 carbon steel coupon as test materials.The sample wherein used all needs to polish step by step through abrasive paper for metallograph, then through the ultrasonic oil removing of acetone, washes of absolute alcohol, cold wind dries up, and is placed in moisture eliminator more than 24 hours, for subsequent use.
Concrete mensuration mode is as follows: be vertically entirely dipped in by A3 carbon steel coupon sample in each testing liquid (comprise the blank ammoniumsulphate soln that do not add inhibiting solution and add the ammoniumsulphate soln after inhibiter) after weighing, lacing film 48h carries out corrosion test (zero-G test in 48 hours, 40 DEG C), sample is taken out after off-test, now can the sample taken out be taken pictures, and by the process of GB6384-86 method, weigh, by the erosion rate of following formula corresponding calculating A3 carbon steel coupon in each testing liquid:
The density checking in soft steel from " alloy mark sheet " is 7.86g/cm
3, then
And then according to following formulae discovery corrosion inhibition rate:
In formula: V
0---the erosion rate (mm/a) of steel sample in the blank ammoniumsulphate soln system not adding inhibiting solution,
V
1---the erosion rate of steel sample after adding inhibiter (mm/a)
The corrosion mitigating effect of table 3A3 carbon steel coupon after adding the inhibiter of embodiment 1-9
(2) by the inhibiter of embodiment 1 according to 0.05wt%, the add-on of 0.1wt%, 0.2wt% joins in 15% ammoniumsulphate soln respectively, then joins in this solution by test materials A3 carbon steel coupon, adopt above-mentioned weight-loss method to measure its corrosion inhibition, the results are shown in Figure 1 and table 4.
Result is as follows: A3 carbon steel coupon 15% ammonium sulfate (empty from system), after zero-G test in 48 hours steel sample apparent dimmed, obviously corrode, as shown in Fig. 1 (a), and as calculated erosion rate be 0.61mm/a.
A3 carbon steel coupon in 15% ammoniumsulphate soln of inhibiter adding 0.05wt% embodiment 1, after zero-G test in 48 hours steel sample apparent very well, still have metalluster, as Fig. 1 (b).And as calculated: its erosion rate is 0.058mm/a, and then must corrosion inhibition rate be 90.5%.
A3 carbon steel coupon in 15% ammoniumsulphate soln of inhibiter adding 0.1wt% embodiment 1, after zero-G test in 48 hours steel sample apparent very well, still have metalluster, as Fig. 1 (c).And as calculated: its erosion rate is 0.048mm/a, and then must corrosion inhibition rate be 92.1%;
A3 carbon steel coupon in 15% ammoniumsulphate soln of inhibiter adding 0.2wt% embodiment 1, after zero-G test in 48h hour steel sample apparent very well, still have metalluster, as Fig. 1 (d).And as calculated: its erosion rate is 0.041mm/a, and then must corrosion inhibition rate be 93.3%;
Table 4 adds the corrosion mitigating effect of the inhibiter of the embodiment of different amounts
(3) corrosion inhibition of inhibiter in the ammoniumsulphate soln system of different concns:
It is in the ammoniumsulphate soln system of 5%, 10% and 30% that the inhibiter of embodiment 1 is all joined concentration respectively according to the add-on of 0.2wt%, then test materials A3 carbon steel coupon is joined in this solution, adopt above-mentioned weight-loss method to measure its corrosion inhibition, the results are shown in Table 5.
The corrosion mitigating effect of inhibiter in the ammoniumsulphate soln of different concns of table 5 embodiment 1
(4) inhibiter of embodiment 1 is joined in ammonia process of desulfurization Sulphuric acid ammonium solution (being taken to Wuhan Sulphuric acid ammonium factory) according to the add-on of 0.2wt%, then test materials A3 carbon steel coupon is put into the (zero-G test in 48 hours of lacing film 48h in this solution, 40 DEG C), above-mentioned weight-loss method is adopted to measure its corrosion inhibition, result table 6.
Corrosion mitigating effect in the ammonia process of desulfurization Sulphuric acid ammonium solution of table 6A3 carbon steel coupon after adding different inhibiter
Claims (6)
1. suppress the inhibiter that carbon steel corrodes in ammonia process of desulfurization Sulphuric acid ammonium system, it is characterized in that: it is made up of thiourea derivative, organic amine and imidazoline quaternary ammonium salt, wherein the content of each component is by weight percentage: thiourea derivative 20% ~ 80%; Organic amine 10% ~ 50%; Imidazoline quaternary ammonium salt 5% ~ 40%;
Described thiourea derivative is selected from the one in phenylthiourea, diphenyl thiourea, thiosemicarbazide and Allyl thiourea;
Described organic amine is selected from the one in polyacrylamide, amino dodecane, cetylamine and stearylamine;
The chemical structural formula of described imidazoline quaternary ammonium salt is:
Wherein, R is phenyl, C2-C11 straight chained alkyl, CH
3(CH
2)
7cH=CH (CH
2)
7or CH
3(CH
2)
9cH=CH (CH
2)
7; N value is 2,3 or 4.
2. the inhibiter that corrodes in ammonia process of desulfurization Sulphuric acid ammonium system of suppression carbon steel according to claim 1, is characterized in that: the content of described each component is by weight percentage: thiourea derivative 65% ~ 75%; Organic amine 15% ~ 25%; Imidazoline quaternary ammonium salt 5% ~ 15%.
3. the inhibiter that corrodes in ammonia process of desulfurization Sulphuric acid ammonium system of suppression carbon steel according to claim 1, it is characterized in that: described imidazoline quaternary ammonium salt is commercial commercialization imidazoline quaternary ammonium salt, or make by oneself by the following method, concrete preparation method is as follows: by organic carboxyl acid RCOOH, wherein: R is phenyl, C2-C11 straight chained alkyl, CH
3(CH
2)
7cH=CH (CH
2)
7or CH
3(CH
2)
9cH=CH (CH
2)
7, and polyethylene polyamine NH
2cH
2cH
2nH (CH
2cH
2nH)
n-1h, wherein: n value is 2,3 or 4, joins in reaction vessel according to the molar ratio of 0.5 ~ 1:1, by dimethylbenzene: the mol ratio of organic carboxyl acid=50 ~ 300:1, add dimethylbenzene as azeotropic agent, 130 ~ 170 DEG C of reaction 0.5 ~ 3h, are then warmed up to 180 ~ 240 DEG C, after reaction 2 ~ 3h, cool to 50 DEG C, then dropwise drip Benzyl Chloride wherein while stirring, the mol ratio of described Benzyl Chloride and polyethylene polyamine is 1 ~ 1.5:1, control temperature is 90 ~ 110 DEG C again, reacts 1 ~ 3h and get final product.
4. the suppression carbon steel according to claim 1 using method of inhibiter of corroding in ammonia process of desulfurization Sulphuric acid ammonium system, is characterized in that: it comprises the following steps:
(1) thiourea derivative in inhibiter is mixed with the thiourea derivative aqueous solution;
(2) organic amine in inhibiter is mixed with organic amine ethanolic soln;
(3) imidazoline quaternary ammonium salt in inhibiter is mixed with imidazoline quaternary ammonium salt ethanolic soln;
(4) according to the consumption requirement of inhibiter, and in conjunction with the proportioning of component each in inhibiter, obtain the consumption of each component, then get the solution of each component of respective volume accordingly, join ammonia process of desulfurization Sulphuric acid ammonium system simultaneously, stir.
5. the suppression carbon steel according to claim 4 using method of inhibiter of corroding in ammonia process of desulfurization Sulphuric acid ammonium system, is characterized in that: the mass percent concentration of the described thiourea derivative aqueous solution is 0.5%-5%; The mass percent concentration of described organic amine ethanolic soln is 0.5%-5%; The mass percent concentration of described imidazoline quaternary ammonium salt ethanolic soln is 40%-60%.
6. the suppression carbon steel according to claim 4 using method of inhibiter of corroding in ammonia process of desulfurization Sulphuric acid ammonium system, is characterized in that: during use, the mass percent concentration of described inhibiter is 0.05 ~ 0.2%.
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| CN110344063A (en) * | 2019-08-27 | 2019-10-18 | 山东益丰生化环保股份有限公司 | A kind of modified imidazoline corrosion inhibiter and preparation method thereof |
| CN110747002B (en) * | 2019-11-13 | 2021-06-15 | 上海贵通新材料科技有限公司 | Coking corrosion inhibitor |
| CN113005462B (en) * | 2019-12-20 | 2023-03-24 | 齐鲁工业大学 | Descaling and cleaning corrosion inhibitor and cleaning agent for 201 stainless steel |
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| US6866797B1 (en) * | 2000-08-03 | 2005-03-15 | Bj Services Company | Corrosion inhibitors and methods of use |
| CN101613622B (en) * | 2009-07-29 | 2012-08-22 | 中国石油化工集团公司 | Composite inhibiter and preparation method and application thereof |
| CN102321463A (en) * | 2011-06-14 | 2012-01-18 | 北京科技大学 | Sulfur-containing bis-imidazoline type carbon dioxide corrosion inhibitor and preparation method thereof |
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