CN114807948B - Method for conveniently preparing pickling solution containing carbon dot corrosion inhibitor - Google Patents
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- 230000007797 corrosion Effects 0.000 title claims abstract description 66
- 238000005260 corrosion Methods 0.000 title claims abstract description 66
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 54
- 239000003112 inhibitor Substances 0.000 title claims abstract description 53
- 238000005554 pickling Methods 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 87
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 150000001413 amino acids Chemical class 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000010790 dilution Methods 0.000 claims abstract description 8
- 239000012895 dilution Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 235000001014 amino acid Nutrition 0.000 claims description 16
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims description 9
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 9
- 235000018417 cysteine Nutrition 0.000 claims description 9
- 235000013922 glutamic acid Nutrition 0.000 claims description 9
- 239000004220 glutamic acid Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 3
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims description 3
- 239000004475 Arginine Substances 0.000 claims description 2
- 239000004471 Glycine Substances 0.000 claims description 2
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims description 2
- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 claims description 2
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 claims description 2
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-UHFFFAOYSA-N 0.000 claims description 2
- 235000004279 alanine Nutrition 0.000 claims description 2
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 claims description 2
- 235000009697 arginine Nutrition 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 13
- 229910000975 Carbon steel Inorganic materials 0.000 abstract description 11
- 239000010962 carbon steel Substances 0.000 abstract description 11
- 230000005764 inhibitory process Effects 0.000 abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 7
- 238000004140 cleaning Methods 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010000 carbonizing Methods 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 239000010949 copper Substances 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract description 2
- 229910000851 Alloy steel Inorganic materials 0.000 abstract 1
- -1 carbon steel Chemical class 0.000 abstract 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 238000006386 neutralization reaction Methods 0.000 description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 238000007112 amidation reaction Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000005536 corrosion prevention Methods 0.000 description 2
- 238000002481 ethanol extraction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000002390 rotary evaporation Methods 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- WUBBRNOQWQTFEX-UHFFFAOYSA-N 4-aminosalicylic acid Chemical compound NC1=CC=C(C(O)=O)C(O)=C1 WUBBRNOQWQTFEX-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229960004909 aminosalicylic acid Drugs 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine powder Natural products NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention discloses a method for conveniently preparing pickling solution containing carbon spot corrosion inhibitors, which comprises the following specific steps: adding water into raw materials of the carbon dot corrosion inhibitor by taking amino acid as raw materials, and stirring to disperse the amino acid in the water to obtain an amino acid solution; adding concentrated sulfuric acid with the concentration not lower than 95% into the obtained amino acid solution, and stirring uniformly while adding; uniformly heating the obtained mixed solution at 50-90 ℃ for 20-300 min, and dehydrating and carbonizing amino acid in the solution under the action of concentrated sulfuric acid; and pouring the obtained reacted solution into water for dilution, and stirring while pouring, wherein the obtained diluted solution is the pickling solution containing the carbon dot corrosion inhibitor. The method is simple and convenient, and can realize the large-scale preparation of the pickling solution containing the carbon dot corrosion inhibitor. More importantly, the prepared carbon dots are doped with nitrogen elements, so that the corrosion inhibition effect is stronger, and under the protection of the carbon dot corrosion inhibitor, the pickling solution can be used for efficiently cleaning metals such as carbon steel, low alloy steel, copper and the like without damaging metal matrixes.
Description
Technical Field
The invention relates to the field of preparation and application of functional materials, in particular to a method for conveniently preparing pickling solution containing carbon spot corrosion inhibitors.
Background
Carbon dots were first discovered in 2004 and were defined as carbon nanoparticles with fluorescent effect, typically less than 10nm in size. Most carbon sites consist of two parts, a core, which is typically composed of sp2 hybridized graphitic carbon or amorphous carbon, and a surface group, which is mostly an oxygen-containing or nitrogen-containing group. The fluorescent dye has the advantages of unique fluorescence adjustability, excellent light stability, small size effect, good biocompatibility, excellent catalytic property, low toxicity, environmental protection and the like, and is widely applied to the fields of chemical sensing, biological imaging, catalysis, photoelectric devices, plant systems, lubrication, corrosion prevention and the like.
The carbon dots are applied in the field of corrosion prevention and start later. In 2017, researchers have explored the application of carbon dots in the field of corrosion protection for the first time. Specifically, the antibiotic aminosalicylic acid is used as a raw material, nitrogen-doped carbon dots with high water solubility and low cytotoxicity are prepared by a hydrothermal method, and the nitrogen-doped carbon dots are used as environment-friendly corrosion inhibitors for inhibiting corrosion of carbon steel in a hydrochloric acid solution with the concentration of 1M, and the slow release efficiency is as high as 96%. According to the inspired by the method, some researchers prepare various carbon points with different types, and the carbon points are used as corrosion inhibitors of metals such as copper, carbon steel, aluminum and the like, and the corrosion inhibitors show excellent corrosion resistance in acid solution and sodium chloride neutral solution, and the optimal corrosion inhibition efficiency is higher than 90%. At present, a great deal of researches prove that the nitrogen doped carbon point can better form a protective film through the chemical adsorption action of nitrogen and metal elements due to the inclusion of nitrogen element, so as to protect the metal matrix from being corroded by pickling solution.
Based on this, document CN111662243a discloses a citric acid-based functionalized carbon dot corrosion inhibitor, and a preparation method and application thereof. The citric acid functional carbon dot corrosion inhibitor is prepared by carrying out hydrothermal reaction on citric acid in the presence of deionized water, respectively adding deionized water, absolute ethyl alcohol and triethylamine after cooling reaction liquid, stirring, then adding 4-dimethylaminopyridine, adding melamine powder after stirring and dissolving, stirring and then heating for amidation reaction. The carbon dot corrosion inhibitor has nitrogen element due to amidation reaction, and has higher efficient corrosion inhibition performance.
The carbon dot corrosion inhibitor prepared by the document still has the defects of environmental protection, low preparation efficiency, expensive raw materials and the like. In addition, if the carbon dot corrosion inhibitor is used as a corrosion inhibitor of pickling solution, the prepared carbon dot corrosion inhibitor is added into an acid solution, and then stirred and mixed, so that the pickling solution containing the carbon dot corrosion inhibitor can be obtained, and the process is complicated.
Disclosure of Invention
The invention aims to provide a convenient, efficient and low-cost method for preparing the pickling solution containing the carbon dot corrosion inhibitor in one step, aiming at the problems that the existing method for preparing the carbon dot corrosion inhibitor is not environment-friendly, low in preparation efficiency, expensive in raw materials, incapable of obtaining the pickling solution containing the carbon dot corrosion inhibitor in one step and the like.
The technical scheme of the invention is as follows:
a method for conveniently preparing pickling solution containing carbon point corrosion inhibitors comprises the following steps:
step one: adding water into raw materials of the carbon dot corrosion inhibitor by taking amino acid as raw materials, and stirring to disperse the amino acid in the water to obtain an amino acid solution;
step two: adding concentrated sulfuric acid with the concentration not lower than 95% into the amino acid solution obtained in the step one, and uniformly stirring while adding to prevent the concentrated sulfuric acid from generating a bumping phenomenon;
step three: uniformly heating the mixed solution obtained in the second step at 50-90 ℃ for 20-300 min, and dehydrating and carbonizing amino acid in the solution under the action of concentrated sulfuric acid, wherein the color of the solution is changed from colorless to yellow, brown or brown and the like, so that a new substance, namely carbon dots, is generated, and the carbon dots are nitrogen-doped carbon dots due to the fact that the used amino acid contains nitrogen, so that the corrosion inhibition effect is higher;
step four: and (3) pouring the solution obtained after the reaction in the step (III) into water for dilution, stirring while reversing to prevent the concentrated sulfuric acid from generating a bumping phenomenon, and uniformly stirring to obtain a diluted solution which is the pickling solution of the carbon point-containing corrosion inhibitor.
The method for conveniently preparing the pickling solution containing the carbon dot corrosion inhibitor comprises the following steps that the amino acid in the first step is one or more of tryptophan, cysteine, glycine, alanine, arginine and glutamic acid.
According to the method for conveniently preparing the pickling solution containing the carbon dot corrosion inhibitor, the mass of the amino acid in the first step accounts for 0.3-5% of the mass of the diluted solution obtained in the third step.
According to the method for conveniently preparing the pickling solution containing the carbon dot corrosion inhibitor, the mass of the concentrated sulfuric acid added in the second step is 4 times that of the water added in the first step, so that the concentrated sulfuric acid can effectively enable the amino acid to undergo a dehydration carbonization reaction, and nitrogen-doped carbon dots can be efficiently generated.
According to the method for conveniently preparing the pickling solution containing the carbon dot corrosion inhibitor, in the third step, the mass of the water used for dilution is added according to the mass fraction of the concentrated sulfuric acid, so that the mass fraction of the sulfuric acid contained in the obtained diluted solution, namely the pickling solution containing the carbon dot corrosion inhibitor, is in the range of 5-20%.
The beneficial effects of the invention are as follows: (1) environmental protection without harmful substances; (2) The cost is low, the preparation efficiency is high, and the pickling solution containing the carbon point corrosion inhibitor can be prepared in situ in one step; (3) is suitable for large-scale production.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention.
FIG. 2 is a Transmission Electron Microscope (TEM) image of the carbon dot corrosion inhibitor in the pickling solution prepared in example 1.
FIG. 3 is a TEM image of the carbon dot corrosion inhibitor in the pickling solution prepared in example 2.
In the figure: S1-S4 correspond to steps one to four of the method.
Detailed Description
The following are 2 specific embodiments of the present invention, and the technical solution of the present invention is further described with reference to the accompanying drawings. Glutamic acid, cysteine, concentrated sulfuric acid and the like used in the examples were purchased from chemical reagent limited of national pharmaceutical group and were used directly without purification treatment for analytical grade.
Example 1
As shown in FIG. 1, the method for conveniently preparing the pickling solution containing the carbon dot corrosion inhibitor comprises the following specific steps:
step one: 0.4g of glutamic acid is taken as a raw material of the carbon point corrosion inhibitor, 0.8mL of deionized water is added and stirred, so that the glutamic acid is dispersed in water to obtain a glutamic acid solution;
step two: adding 4mL of 98% concentrated sulfuric acid into the glutamic acid solution obtained in the step one, and stirring uniformly while adding so as to prevent the concentrated sulfuric acid from generating a bumping phenomenon;
step three: heating the mixed solution obtained in the second step at 75 ℃ for 150min, and carrying out dehydration carbonization reaction on glutamic acid in the solution under the action of concentrated sulfuric acid, wherein the color of the solution is changed from colorless to yellow, so that a new substance, namely carbon dots, is generated, and the carbon dots are nitrogen-doped carbon dots due to the fact that the used glutamic acid contains nitrogen, so that the corrosion inhibition effect is higher;
step four: and D, pouring the solution obtained after the reaction in the step three into deionized water for dilution, stirring while reversing to prevent the concentrated sulfuric acid from generating a bumping phenomenon, wherein the volume of the used dilution water is 74mL, and stirring uniformly to obtain the diluted solution which is the pickling solution containing the carbon dot corrosion inhibitor. The mass fraction of concentrated sulfuric acid in the pickling solution is about 5%, and no other additives are added.
To demonstrate that nitrogen-doped carbon dots were formed in the prepared pickling solution, the obtained pickling solution was subjected to operations such as neutralization (sodium hydroxide solution as a neutralization solution), rotary evaporation, ethanol extraction, freeze drying, and the like, to obtain a solid product, which was subjected to TEM characterization (fig. 2), and the product was a nearly circular black dot having an average particle diameter of about 6.8nm, and the carbon dots were determined to be formed, and further the carbon dots were verified to contain N element using X-ray photoelectron spectroscopy, and thus the nitrogen-doped carbon dots were determined to be formed.
In order to prove the corrosion inhibition effect of the nitrogen-doped carbon point corrosion inhibitor and the cleaning effect of the pickling solution, the prepared pickling solution containing the carbon point corrosion inhibitor and concentrated sulfuric acid (5%) with the same concentration are used for a Q235 carbon steel rust removal experiment (1 cm x 0.3cm Q235 carbon steel blocks under the same rust generation condition are respectively soaked in the two pickling solutions for 3 hours). The result shows that the concentrated sulfuric acid (5%) pickling solution with the same concentration does not contain carbon dot corrosion inhibitor, so that the Q235 carbon steel matrix is greatly corroded, and the surface is uneven; the pickling solution containing the carbon dot corrosion inhibitor prepared in the embodiment 1 only removes rust on the surface of the Q235 carbon steel, and does not corrode a matrix, so that the surface is flat and smooth. Therefore, the corrosion inhibition effect of the carbon dot corrosion inhibitor and the cleaning effect of the prepared pickling solution are proved.
Example 2
A method for conveniently preparing pickling solution containing carbon point corrosion inhibitors comprises the following specific steps:
step one: 0.4g of cysteine is taken as a raw material of the carbon dot corrosion inhibitor, 0.8mL of deionized water is added and stirred, so that the cysteine is dispersed in the water to obtain a cysteine solution;
step two: adding 4mL of concentrated sulfuric acid with the concentration of 98% into the cysteine solution obtained in the step one, and uniformly stirring while adding to prevent the concentrated sulfuric acid from generating a bumping phenomenon;
step three: heating the mixed solution obtained in the second step at 70 ℃ for 150min, and carrying out dehydration carbonization reaction on cysteine in the solution under the action of concentrated sulfuric acid, wherein the color of the solution is changed from colorless to yellow, so that a new substance, namely carbon dots, is generated, and the carbon dots are nitrogen-doped carbon dots due to the fact that the used cysteine contains nitrogen, so that the corrosion inhibition effect is higher;
step four: and D, pouring the solution obtained after the reaction in the step three into deionized water for dilution, stirring while reversing to prevent the concentrated sulfuric acid from generating a bumping phenomenon, wherein the volume of the used dilution water is 74mL, and stirring uniformly to obtain the diluted solution which is the pickling solution containing the carbon dot corrosion inhibitor. The mass fraction of concentrated sulfuric acid in the pickling solution is about 5%, and no other additives are added.
To demonstrate that nitrogen-doped carbon dots were formed in the prepared pickling solution, the obtained pickling solution was subjected to operations such as neutralization (sodium hydroxide solution as a neutralization solution), rotary evaporation, ethanol extraction, freeze drying, and the like, to obtain a solid product, which was subjected to TEM characterization (fig. 3), and the product was a nearly circular black dot having a particle diameter of 10nm or less, and the carbon dots were determined to be formed, and further the carbon dots were verified to contain N element using X-ray photoelectron spectroscopy, thereby determining that nitrogen-doped carbon dots were formed.
In order to prove the corrosion inhibition effect of the nitrogen-doped carbon point corrosion inhibitor and the cleaning effect of the pickling solution, the prepared pickling solution containing the carbon point corrosion inhibitor and concentrated sulfuric acid (5%) with the same concentration are used for a Q235 carbon steel rust removal experiment (1 cm x 0.3cm Q235 carbon steel blocks under the same rust generation condition are respectively soaked in the two pickling solutions for 3 hours). The result shows that the concentrated sulfuric acid (5%) pickling solution with the same concentration does not contain carbon dot corrosion inhibitor, so that the Q235 carbon steel matrix is greatly corroded, and the surface is uneven; the pickling solution containing the carbon dot corrosion inhibitor prepared in the embodiment 2 only removes rust on the surface of the Q235 carbon steel, and does not corrode a matrix, so that the surface is flat and smooth. Therefore, the corrosion inhibition effect of the carbon dot corrosion inhibitor and the cleaning effect of the prepared pickling solution are proved.
Claims (2)
1. A method for conveniently preparing pickling solution containing carbon point corrosion inhibitors is characterized by comprising the following steps:
step one: adding water into raw materials of the carbon dot corrosion inhibitor by taking amino acid as raw materials, and stirring to disperse the amino acid in the water to obtain an amino acid solution;
step two: adding concentrated sulfuric acid with the concentration not lower than 95% into the amino acid solution obtained in the step one, and stirring uniformly while adding so that the mass of the added concentrated sulfuric acid is 4 times greater than that of water added in the step one;
step three: uniformly heating the mixed solution obtained in the step two at 50-90 ℃ for 20-300 min, and carrying out dehydration carbonization reaction on amino acid in the solution under the action of concentrated sulfuric acid;
step four: and (3) pouring the solution obtained after the reaction in the step (III) into water for dilution, and stirring while reversing, so that the mass fraction of sulfuric acid contained in the obtained diluted solution ranges from 5% to 20%, the mass fraction of amino acid contained in the diluted solution ranges from 0.3% to 5%, and the obtained diluted solution is the pickling solution containing the carbon point corrosion inhibitor.
2. The method for preparing pickling solution containing carbon point corrosion inhibitors conveniently according to claim 1, wherein the amino acid in the step one is one or more of tryptophan, cysteine, glycine, alanine, arginine and glutamic acid.
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DE10043040A1 (en) * | 2000-09-01 | 2002-03-28 | Goldschmidt Ag Th | Use of N-alkyl-beta-alanine derivatives for the production of cleaning anti-corrosion agents |
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Title |
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A novel fluorescent sensor based on sulfur and nitrogen co-doped carbon dots with excellent stability for selective detection of doxycycline in raw milk;Jinping Song et al.;RSC Adv.;第7卷;1-8 * |
Carbon dots as new eco-friendly and effective corrosion inhibitor;Mingjun Cui et al.;Journal of Alloys and Compounds;第726卷;680-692 * |
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