CN112442694A - Magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor and preparation method and application thereof - Google Patents
Magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor and preparation method and application thereof Download PDFInfo
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- CN112442694A CN112442694A CN201910817501.1A CN201910817501A CN112442694A CN 112442694 A CN112442694 A CN 112442694A CN 201910817501 A CN201910817501 A CN 201910817501A CN 112442694 A CN112442694 A CN 112442694A
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- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
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Abstract
The invention discloses a magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor and a preparation method thereof. The compound sustained release agent (Fe)3O4/CS/Inhibitors) is based on the load capacity of chitosan, Fe3O4The superparamagnetic performance and the synergistic effect of the two corrosion inhibitors of sodium molybdate and sodium benzoate are used for a seawater circulating cooling system for a long time and efficiently, the effects of targeted positioning, magnetic control release and efficient corrosion inhibition are achieved, and further the corrosion resistance and the service life of the carbon steel in seawater are improved.
Description
Technical Field
The invention relates to the technical field of seawater circulating cooling, in particular to a magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor, and a preparation method and application thereof.
Background
The seawater circulating cooling technology is an important technology which uses seawater as a cooling medium instead of fresh water so as to save fresh water resources and reasonably and efficiently utilize seawater resources. The low-carbon steel has the advantages of good processing performance, low cost and the like, and is widely applied to a seawater circulating cooling system. However, severe corrosion of mild steel has largely limited its application.
In several methods for inhibiting the corrosion of low-carbon steel, the addition of the corrosion inhibitor is an effective way for efficiently slowing down the corrosion rate at low cost. However, the addition of a large amount of corrosion inhibitor causes resource waste, environmental pollution, short-term effect and the like.
In recent years, in order to reduce the waste of the corrosion inhibitor and realize the slow release and long-term action of the corrosion inhibitor, the corrosion inhibitor is usually loaded in a nano container such as mesoporous silica nanoparticles or layered double hydroxides (hydrotalcites). The interaction force between the corrosion inhibitor and the nano container is utilized, so that the sustained release of the corrosion inhibitor is realized. However, the method has the disadvantages of complex preparation process, low corrosion inhibitor loading capacity and the like.
Chitosan (CS) is a product of chitosan deacetylation, is a natural polysaccharide composed of most of D-glucosamine and a small amount of N-acetyl-D-glucosamine, has the characteristics of biocompatibility, biodegradability, low cost, nontoxicity, and the like, and is widely used in the medical field.
The chitosan has higher loading capacity, and is particularly simple in preparation process compared with other carriers. Therefore, it is feasible to encapsulate the corrosion inhibitor into the magnetic chitosan nanoparticles to prepare the novel composite corrosion inhibitor. The corrosion inhibitor can be brought to a target place, the release rate of the corrosion inhibitor can be regulated and controlled through an external magnetic field, and the corrosion inhibitor is quickly recovered to reduce the pollution to the environment.
Disclosure of Invention
The invention aims to solve the problem of corrosion of metal equipment in a seawater circulating cooling system in the prior art, and provides a magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor and a preparation method thereof. The compound sustained release agent (Fe)3O4/CS/Inhibitors) is based on the load capacity of chitosan, Fe3O4The superparamagnetic performance and the synergistic effect of the two corrosion inhibitors of sodium molybdate and sodium benzoate are used for a seawater circulating cooling system for a long time and efficiently, the effects of targeted positioning, magnetic control release and efficient corrosion inhibition are achieved, and further the corrosion resistance and the service life of the carbon steel in seawater are improved.
The technical scheme adopted for realizing the purpose of the invention is as follows:
a preparation method of a magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor comprises the following steps:
step 1: preparing glacial acetic acid solution of chitosan, and adding sodium molybdate dihydrate, sodium benzoate and Fe3O4Uniformly dispersing to obtain suspension A;
step 2: preparing TPP aqueous solution, and uniformly dispersing to obtain solution B;
and step 3: dropwise adding the solution B into the suspension A, and mechanically stirring for 2-6h after dropwise adding is finished to obtain reaction slurry;
and 4, step 4: separating the obtained reaction slurry with a permanent magnet, centrifugally washing the reaction slurry with absolute ethyl alcohol to be neutral, drying and grinding the reaction slurry to obtain Fe3O4/CS/Inhibitors。
In the preparation method, the concentration of the glacial acetic acid solution of the chitosan is 1.0mg/mL-6.0 mg/mL.
In the above preparation method, in step 1, chitosan, sodium molybdate dihydrate, sodium benzoate and Fe3O4The mass ratio of (6-36): (20-120): (20-120): (6-12).
In the above preparation method, in step 1, chitosan, sodium molybdate dihydrate, sodium benzoate and Fe3O4The mass ratio of (12-36): (40-80): (40-80): (8-10).
In the above preparation method, in step 1, chitosan, sodium molybdate dihydrate, sodium benzoate and Fe3O4The mass ratio of (A) to (B) is 3: 10: 10: 2.
in the above preparation method, the concentration of the TPP solution in step 2 is 0.375mg/mL-3.000 mg/mL.
In the preparation method, in the step 2, the mass ratio of TPP to chitosan in the step 1 is 1: (2-8).
In the preparation method, in the step 4, the drying method is drying for 6-24h in a drying oven at 50-90 ℃.
The magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor prepared by the preparation method.
The magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor is applied to a seawater circulating cooling system.
Compared with the prior art, the invention has the beneficial effects that:
the composite corrosion inhibitor provided by the invention takes chitosan as a carrier and utilizes Fe3O4The superparamagnetism and the synergistic effect of the two corrosion inhibitors have the advantages of targeting positioning, magnetic control release and long-term and efficient corrosion inhibition.
Drawings
FIG. 1 is a graph showing the release profile of Fe3O4/CS/Inhibitors in a 3.5% NaCl solution.
Wherein, 1, the release curve of sodium benzoate under no magnetic field; 2. release curve of sodium molybdate in no magnetic field; 3. the release curve of sodium benzoate under a magnetic field; 4. release profile of sodium molybdate under magnetic field.
FIG. 2 is a Nyquist plot of Q235 steel in 3.5% NaCl solution.
FIG. 3 is a Nyquist plot of Q235 steel in 3.5% NaCl +2g/L Fe3O4/CS/Inhibitors solution.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor is prepared according to the following steps:
step 1: weighing 2.7g FeCl3 & 6H2O and 7.2g CH3COONa & 3H2O, dissolving in 60ml ethylene glycol, stirring to form a uniform yellow solution, dropwise adding 1ml polyethylene glycol, continuously stirring uniformly, transferring to a 100ml reaction kettle, and placing the reaction kettle in a 160 ℃ vacuum drying oven for reaction for 12 hours. And separating the obtained product by using a magnet, sequentially centrifuging and washing the product for 3 times by using ethanol and deionized water, drying the product for 24 hours in a drying box at the temperature of 60 ℃, and grinding the product to obtain Fe3O 4.
Step 2: 60mg of chitosan was dissolved in glacial acetic acid (w/v ═ 1%) to prepare 60mL of a 1.0mg/mL chitosan solution, and then 0.2g of sodium molybdate dihydrate and 0.2g of sodium benzoate were added to the above chitosan solution.
And step 3: 0.06g of Fe3O4 was weighed out and dispersed in ultrapure water, sonicated for 60min, Fe3O4 was separated with a magnet, redispersed in 60ml of the above chitosan solution, and mechanically stirred at room temperature to obtain suspension A.
And 4, step 4: and m (CS)/m (TPP) ═ 2: 1, TPP was quantitatively weighed and prepared into a TPP solution having a concentration of 0.375mg/ml, referred to as solution B.
And 5: dropwise adding the solution B into the suspension A, and mechanically stirring for 4 hours after the dropwise addition is finished.
Step 6: and separating the obtained reaction slurry by using a permanent magnet, centrifugally washing the reaction slurry to be neutral by using absolute ethyl alcohol, drying the reaction slurry for 24 hours in a drying oven at the temperature of 50 ℃, and grinding the reaction slurry to obtain the magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor.
Example 2
Step 1: weighing 1.2g of FeCl3 & 6H2O and 3.6g of CH3COONa & 3H2O, dissolving in 60ml of ethylene glycol, stirring to form a uniform yellow solution, dropwise adding 1ml of polyethylene glycol, continuously stirring uniformly, transferring to a 100ml reaction kettle, and placing the reaction kettle in a vacuum drying oven at 180 ℃ for reaction for 10 hours. And separating the obtained product by using a magnet, sequentially centrifuging and washing the product for 3 times by using ethanol and deionized water, drying the product for 8 hours in a drying box at the temperature of 60 ℃, and grinding the product to obtain Fe3O 4.
Step 2: a quantitative amount of chitosan was weighed and dissolved in glacial acetic acid (w/v ═ 1%) to prepare 60mL of a 2.0mg/mL chitosan solution, and then 0.8g of sodium molybdate dihydrate and 0.8g of sodium benzoate were weighed and added to the above chitosan solution.
And step 3: 0.10g of Fe3O4 was weighed out and dispersed in ultrapure water, sonicated for 60min, Fe3O4 was separated with a magnet, redispersed in 60ml of the above chitosan solution, and mechanically stirred at room temperature to obtain suspension A.
And 4, step 4: and m (CS)/m (TPP) ═ 3: TPP was weighed out in a fixed amount at a ratio of 1 to prepare a TPP solution having a concentration of 0.750mg/ml, referred to as a B solution.
And 5: dropwise adding the solution B into the suspension A, and mechanically stirring for 2 hours after the dropwise addition is finished.
Step 6: and separating the obtained reaction slurry by using a permanent magnet, centrifugally washing the reaction slurry to be neutral by using absolute ethyl alcohol, drying the reaction slurry for 6 hours in a drying oven at the temperature of 70 ℃, and grinding the reaction slurry to obtain the magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor.
Example 3
Step 1: weighing 3.6g FeCl3 & 6H2O and 9.8g CH3COONa & 3H2O, dissolving in 60ml ethylene glycol, stirring to form a uniform yellow solution, dropwise adding 1ml polyethylene glycol, continuously stirring uniformly, transferring to a 100ml reaction kettle, and placing the reaction kettle in a vacuum drying oven at 200 ℃ for reaction for 16 hours. And separating the obtained product by using a magnet, sequentially centrifuging and washing the product for 3 times by using ethanol and deionized water, drying the product for 12 hours in a drying box at the temperature of 80 ℃, and grinding the product to obtain Fe3O 4.
Step 2: a fixed amount of chitosan was weighed and dissolved in glacial acetic acid (w/v ═ 1%) to prepare 60mL of a 3.0mg/mL chitosan solution, and then 1.2g of sodium molybdate dihydrate and 1.2g of sodium benzoate were weighed and added to the above chitosan solution.
And step 3: 0.12g of Fe3O4 was weighed out and dispersed in ultrapure water, sonicated for 60min, Fe3O4 was separated with a magnet, redispersed in 60ml of the above chitosan solution, and mechanically stirred at room temperature to obtain suspension A.
And 4, step 4: and m (CS)/m (TPP) ═ 4: 1, TPP was weighed out in a fixed amount to prepare a TPP solution having a concentration of 1.500mg/ml, referred to as solution B.
And 5: dropwise adding the solution B into the suspension A, and mechanically stirring for 6 hours after the dropwise addition is finished.
Step 6: and separating the obtained reaction slurry by using a permanent magnet, centrifugally washing the reaction slurry to be neutral by using absolute ethyl alcohol, drying the reaction slurry for 12 hours in a drying oven at the temperature of 90 ℃, and grinding the reaction slurry to obtain the magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor.
Example 4
Step 1: weighing 3.0g of FeCl3 & 6H2O and 6.8g of CH3COONa & 3H2O, dissolving in 60ml of ethylene glycol, stirring to form a uniform yellow solution, dropwise adding 1ml of polyethylene glycol, continuously stirring uniformly, transferring to a 100ml reaction kettle, and placing the reaction kettle in a vacuum drying oven at 120 ℃ for reaction for 10 hours. And separating the obtained product by using a magnet, sequentially centrifuging and washing the product for 3 times by using ethanol and deionized water, drying the product for 8 hours in a drying oven at the temperature of 70 ℃, and grinding the product to obtain Fe3O 4.
Step 2: a fixed amount of chitosan was weighed and dissolved in glacial acetic acid (w/v ═ 1%) to prepare 60mL of a 6.0mg/mL chitosan solution, and then 0.8g of sodium molybdate dihydrate and 0.8g of sodium benzoate were weighed and added to the above chitosan solution.
And step 3: 0.08g of Fe3O4 was weighed out and dispersed in ultrapure water, sonicated for 60min, Fe3O4 was separated with a magnet, redispersed in 60ml of the above chitosan solution, and mechanically stirred at room temperature to obtain suspension A.
And 4, step 4: in the formula of m (CS)/m (TPP) ═ 8: 1, TPP was weighed out in a fixed amount to prepare a TPP solution having a concentration of 3.000mg/ml, referred to as a B solution.
And 5: dropwise adding the solution B into the suspension A, and mechanically stirring for 3 hours after the dropwise addition is finished.
Step 6: and separating the obtained reaction slurry by using a permanent magnet, centrifugally washing the reaction slurry to be neutral by using absolute ethyl alcohol, drying the reaction slurry for 18 hours in a drying oven at the temperature of 60 ℃, and grinding the reaction slurry to obtain the magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor.
Example 5
This example is based on the performance test of the composite corrosion inhibitor prepared in example 1.
1. Magnetic controlled release characteristics
Dispersing 0.2g of Fe3O4/CS/Inhibitors in 100ml of 3.5% NaCl solution, and mechanically stirring; after a certain time interval, 2ml of release medium were removed and at the same time fresh 3.5% NaCl solution was added for compensation; the change of the released concentration of the sodium molybdate and the sodium benzoate in the solution with the absence of a magnetic field along with the release time is measured by an ultraviolet-visible spectrophotometer, so that the release curve of the sodium molybdate and the sodium benzoate is obtained, as shown in figure 1. The release profiles of the two corrosion inhibitors have similar trends. With the prolonging of the release time, the amount of the released corrosion inhibitor is increased rapidly firstly, then is increased slowly, and finally reaches an equilibrium state; under the condition of no magnetic field, the release speed of the corrosion inhibitor is relatively high; after the external magnetic field is applied, the release amount of the corrosion inhibitor is reduced in the same release time under the condition of no magnetic field, and the time for the release to reach the balance is prolonged. Therefore, the synthesized magnetic chitosan composite corrosion inhibition material loaded with sodium molybdate and sodium benzoate has obvious sustained release performance and can realize magnetic control release performance.
2. Long-term high-efficiency corrosion inhibition performance
A polished Q235 steel sample (encapsulated with epoxy resin and having an exposed area of 1 cm) was used2) As a working electrode, saturated calomel as a reference electrode and a platinum sheet electrode as a counter electrode, and electrochemical impedance spectra of Q235 steel in pure 3.5% NaCl solution and 3.5% NaCl solution +2g/LFe3O4/CS/Inhibitors (under an applied magnetic field) were measured by using an Autolab 302 electrochemical workstation, as shown in FIGS. 2 and 3. As can be seen from FIG. 2, there is only one time constant in the 3.5% NaCl solution. After the synthesized composite corrosion inhibitor is added, two time constants exist, and the capacitive arc radius of the impedance spectrum is obviously increased, which indicates that a protective film layer is generated on the surface of the carbon steel. Along with the release time from 15min to 1.5h, the capacitive reactance arc radius is increased along with the release time, and the corresponding corrosion inhibition efficiency is also continuously increased. From 1.5H to 48H, the capacitive arc radius decreases, and the corrosion inhibition efficiency decreases, which may be caused by the release of H + added during the preparation process into the solution, but it can be seen that the capacitive arc radius is still much larger than that of the pure NaCl solution. The corrosion inhibition efficiency reaches 94.69 percent when the release time is 1.5h according to impedance fitting calculation. Namely, the synthesized magnetic chitosan composite corrosion inhibitor material loaded with sodium molybdate and sodium benzoate has long-term and efficient corrosion inhibition effect on the corrosion behavior of carbon steel in seawater.
3. Targeting and retrieval performance
Testing of Fe3O4The magnetization curve of/CS/Inhibitors was found to have a saturation magnetization of 8.00emu g-1And has a very small coercive force of 17.55 oe. 0.5g of Fe3O4the/CS/Inhibitors sample is uniformly dispersed in a container filled with deionized water or absolute ethyl alcohol, a magnet is placed beside the container, the sample can be gathered in 10s, the synthesized sample has superparamagnetism, and the target positioning and the rapid recovery can be realized by utilizing an external magnetic field.
The composite corrosion inhibitor of the present invention was prepared according to the present disclosure by adjusting the process parameters and exhibited substantially the same performance as in example 1.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor is characterized by comprising the following steps:
step 1: preparing glacial acetic acid solution of chitosan, and adding sodium molybdate dihydrate, sodium benzoate and Fe3O4Uniformly dispersing to obtain suspension A;
step 2: preparing TPP aqueous solution, and uniformly dispersing to obtain solution B;
and step 3: dropwise adding the solution B into the suspension A, and mechanically stirring for 2-6h after dropwise adding is finished to obtain reaction slurry;
and 4, step 4: separating the obtained reaction slurry with a permanent magnet, centrifugally washing the reaction slurry with absolute ethyl alcohol to be neutral, drying and grinding the reaction slurry to obtain Fe3O4/CS/Inhibitors。
2. The method of claim 1, wherein the concentration of the glacial acetic acid solution of chitosan in step 1 is 1.0mg/mL to 6.0 mg/mL.
3. The method of claim 1, wherein in step 1, chitosan, sodium molybdate dihydrate, sodium benzoate and Fe3O4The mass ratio of (6-36): (20-120): (20-120): (6-12).
4. The method of claim 1, wherein in step 1, chitosan, sodium molybdate dihydrate, sodium benzoate and Fe3O4The mass ratio of (12-36): (40-80): (40-80): (8-10).
5. The method according to claim 1, wherein in step 1, the mass ratio of chitosan, sodium molybdate dihydrate, sodium benzoate and Fe3O4 is 3: 10: 10: 2.
6. the method of claim 1, wherein in step 2, the concentration of the TPP solution is from 0.375mg/mL to 3.000 mg/mL.
7. The method according to claim 1, wherein the mass ratio of TPP to chitosan in step 1 in step 2 is 1: (2-8).
8. The method according to claim 1, wherein the drying method in step 4 is drying in a drying oven at 50-90 ℃ for 6-24 hours.
9. The magnetic chitosan-loaded sodium molybdate/sodium benzoate composite corrosion inhibitor prepared by the preparation method of any one of claims 1 to 8.
10. The use of the magnetic chitosan loaded sodium molybdate/sodium benzoate composite corrosion inhibitor as claimed in claim 9 in a seawater circulating cooling system.
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