CN110607528A - Controllable-release halloysite-supported molybdate corrosion inhibitor and preparation method thereof - Google Patents
Controllable-release halloysite-supported molybdate corrosion inhibitor and preparation method thereof Download PDFInfo
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- CN110607528A CN110607528A CN201810620674.XA CN201810620674A CN110607528A CN 110607528 A CN110607528 A CN 110607528A CN 201810620674 A CN201810620674 A CN 201810620674A CN 110607528 A CN110607528 A CN 110607528A
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- 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
- 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
- C23F11/18—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 using inorganic inhibitors
- C23F11/185—Refractory metal-containing compounds
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Abstract
The invention discloses a controlled-release halloysite-supported molybdate corrosion inhibitor and a preparation method thereof4 2‑Interaction with Ca ions forms insoluble CaMoO at the ends of HNTs4Composite to mitigate MoO in a pipe4 2‑The release speed of the corrosion inhibitor is expected to improve the service life of the corrosion inhibitor through the controlled release behavior of the corrosion inhibitor, so that the corrosion inhibitor can be conveniently and effectively used for corrosion prevention of metal materials, and the effect of releasing the corrosion inhibitor for a long time is achieved.
Description
Technical Field
The invention belongs to the technical field of corrosion inhibitors, and relates to a preparation method of a corrosion inhibitor for metal corrosion prevention, in particular to a controllable-release halloysite-loaded molybdate and a preparation method thereof.
Background
Because of its excellent mechanical properties and suitable processability, metal materials have been widely used in the industries of automobiles, ships, chemical engineering, aerospace, construction and the like. During use, corrosion of metal materials is an inevitable problem, and the corrosion reduces the performance of the materials, wastes resources and energy, and causes huge economic loss, even major accidents (ZahidahKA, Kakooei S, Ismail MC, Raja PB, Halloysite nanotubes as a nanocontainer for a precise coating application: Areview, [ J ] prog. In order to slow down the corrosion of the material, people take many protective measures, mainly including selecting corrosion-resistant material, electrochemical protection, spraying corrosion-resistant coating and adding corrosion inhibitor (Han is thick, Chenjian is sensitive, Huyanjing, Liumin, ocean engineering structure and ship corrosion protection-current situation and trend [ J ], Chinese material development, 2014, 33: 65-75). Among these methods, the addition of a corrosion inhibitor is considered to be the most commonly used method.
In the early stages of corrosion inhibitor research, chromates, phosphates, nitrites, etc. were often used to inhibit corrosion of metals due to their high corrosion inhibition efficiency, but these corrosion inhibitors have been proved to be harmful to the ecological environment since then and are increasingly banned by many countries (Shchukin DG, Zheludkevich M, Yasakau K, Lamaka S, Ferreira MGS,H,Layer-by-Layer assembled nanocontainers for self-healing corrosion protection[J]adv. mater.2006,18: 1672-. At present, more and more attention is being directed to nontoxic or low-pollution corrosion inhibitors, such as molybdate, tungstate, vanadate, silicate, imidazoline, rare earth salt, gluconate, and natural product corrosion inhibitors (Fouda A S, Megahed H, Ead D M, Lanthanides as environmental friendly from depletion of iron in 3.5% NaCl solution [ J],Desalination and Water Treatment,2013,51(16-18):3164-3178)
In recent years, Buchheit, Kendig and the like are based on the idea of active corrosion prevention, and the corrosion inhibitor is encapsulated inside a micro/nano container by a microencapsulation method, so that the controllable release of the corrosion inhibitor is realized, and the aim of long-term release is fulfilled ([ 1)]Kendig M,Hon M,Warren L,‘Smart’corrosion inhibiting coatings[J],Progress in Organic Coatings,2003,47:183-189。[2]ShchukinD G,Lamaka S V,Yasakau K A,Zheludkevich M L,Ferreira M G S,Mohwald H,Active anticorrosion coatings withhalloysite nanocontainers[J]J.Phys.chem.C., 2008,112: 958-964). Currently, a number of micro/nano-containers have been investigated for encapsulating corrosion inhibitors, including mainly polyelectrolyte and polymer microcapsules, porous silica nanoparticles, layered double hydroxides, and Halloysite Nanotubes (HNTs), among others. HNTs (Al)2Si2O5(OH)4·nH2O) is a natural hollow tubular clay mineral,chemical properties similar to kaolinite (Abdulalev E, Price R, Shchukin D, Lvov Y, Halloysite tubes as nanocontainers for antimicrobial coating with benzotriazole [ J)]ACS appl. Mater. interfaces,2009,1: 1437-. When n is 0, called dehydrated halloysite; when n is 2, hydrated halloysite. HNTs have an inner diameter of about 15nm and an outer diameter of about 50nm and a length of 0.5-2 μm (Joo Y, Sim JH, Jeon Y, Lee SU, Sohn D, Opening and blocking the inner-pors of hallosylite [ J ]]chem.Commun.2013,49: 4519-4521). The hollow tubular structure of HNTs makes it a nano-container widely used for drug and corrosion inhibitor loading ([1 ]]Abdullayev E,Sakakibara K,Okamoto K,Wei W,Ariga K,Lvov Y,Natural tubule clay template synthesis of silver nanorods forantibacterial composite coating[J],ACS Appl.Mater.Interfaces,2011,3:4040-4048；[2]Shchukin D,Moehwald H,Self-repairing coating containing active nanoreservoirs[J]Small,2007,3: 926-943). Abdulalev et al, loaded BTA molecules with HNTs, demonstrated that HNTs could prolong BTA release time and achieve sustained release (Abdulalev E, Price R, ShchukinD, Lvov Y, Halloysite tubes as nanocontainers for antimicrobial coating with benzotriazole [ J]，ACS Applied Materials&Interfaces,2009,1(7):1437-1443)。
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a halloysite-loaded molybdate corrosion inhibitor with controllable release and a preparation method thereof4 2-Interaction with Ca ions forms insoluble CaMoO at the ends of HNTs4Composite to mitigate MoO in a pipe4 2-The release speed of the corrosion inhibitor is expected to improve the service life of the corrosion inhibitor through the controlled release behavior of the corrosion inhibitor, so that the corrosion inhibitor can be conveniently and effectively used for corrosion prevention of metal materials, and the effect of releasing the corrosion inhibitor for a long time is achieved.
The technical purpose of the invention is realized by the following technical scheme:
a controlled-release halloysite molybdate corrosion inhibitor is prepared by loading molybdate into HNTs (HNTs) and utilizingMoO of halloysite pipe orifice4 2-Interaction with Ca ions forms insoluble CaMoO at the ports of halloysite4Composite to achieve mitigation of MoO in halloysite tubes4 2-The release rate of (c).
The preparation method of the corrosion inhibitor comprises the following steps:
step 1, dispersing halloysite in an aqueous solution of molybdate to form a suspension, and loading the molybdate into the halloysite in a vacuum environment by using a negative pressure method;
in step 1, the molybdate is sodium molybdate, potassium molybdate or ammonium molybdate.
In step 1, the mass ratio of molybdate to halloysite is (5-15): (2-8), preferably (8-15): (5-8).
In the step 1, the suspension is placed in a vacuum environment, a vacuum pump is used for vacuumizing and maintaining, the vacuum degree is 1000-2000 Pa, the vacuum degree maintaining time is 30-120 min, then the normal pressure is recovered and maintained for 30-60 min, a loading process is completed, and the loading process is repeated for 2-6 times to complete loading of molybdate into the halloysite.
Step 2, dispersing the product prepared in the step 1 into an aqueous solution containing calcium ions, continuously dispersing, and utilizing MoO of a halloysite nozzle4 2-Interaction with Ca ions forms insoluble CaMoO at the ports of halloysite4And (c) a complex.
In step 2, the aqueous solution containing calcium ions is an aqueous solution of calcium chloride, and the mass percent of the calcium chloride is 0.1-6.0 wt%, preferably 2-5 wt%.
In step 2, the continuous dispersion is carried out by using ultrasound or stirring for 1 to 30min, preferably 10 to 30 min.
In step 2, after dispersion is stopped, centrifuging and washing are carried out, drying is carried out for 20-24 h at the temperature of 40-90 ℃, and then grinding is carried out, thus obtaining HNTs loaded molybdate and CaMoO4Encapsulated corrosion inhibitor material (Ca-Na)2MoO4-HNTs)。
Compared with the prior art, the technical scheme of the invention is that molybdate is negatively chargedLoaded into HNTs and using MoO at their ports4 2-Interaction with Ca ions to form CaMoO4The MoO in the pipe can be regulated and controlled after the compound4 2-The release speed of the release agent is controlled to achieve the purpose of controllable release; on the other hand, because of Ca-Na2MoO4The HNTs corrosion inhibitor has the function of long-acting release, so the corrosion inhibitor can play a role of long-term protection on the corrosion prevention of carbon steel, and the service life of the corrosion inhibitor is prolonged.
Drawings
FIG. 1 shows HNTs, Na in the present invention2MoO4-HNTs and Ca-Na2MoO4TEM images of HNTs samples.
FIG. 2 shows HNTs, Na in the present invention2MoO4HNTs and pure Na2MoO4XRD pattern of the crystal.
FIG. 3 is a representation of HNTs, pure CaMoO, of the present invention4And different concentrations of CaCl2Ca-Na obtained after solution treatment2MoO4XRD patterns of HNTs.
FIG. 4 shows CaCl at various concentrations2Ca-Na obtained after solution encapsulation2MoO4MoO of HNTs materials in Water4 2-The release profile.
FIG. 5 shows Q235 steel at 3.5% NaCl and 3.5% NaCl +1g/L Ca-Na2MoO4Nyquist plots of HNTs material in solution at different release times.
Detailed Description
The invention will be further described with reference to the following figures and examples, but the invention is not limited to these specific examples. HNTs are produced by Shanghai City industries, Inc.; na (Na)2MoO4·2H2O and CaCl2Manufactured by Tianjin Yuanhui reagent Co., Ltd; all chemicals were analytically pure.
Example 1
(1) Mixing Na2MoO4·2H2O (8.0g) was dissolved in 100ml of deionized water, and then 4g of HNTs were added thereto to form a suspension, referred to as A suspension.
(2) Transferring the suspension A toA100 ml beaker was then placed in a vacuum canister and evacuated to 1.325E3Pa (1.325X 10) using a vacuum pump3Pa, i.e. 1325Pa) and maintained at this pressure for 90min, and then the system is placed again at atmospheric pressure for 30min, referred to as completing the loading process. The above cycle was repeated and 3 loading experiments were completed.
(3) Centrifuging and washing the sample after 3 times of loading, and then re-dispersing the sample into 5.0 wt% of CaCl2Stirring in the solution for 10min, centrifuging, washing, drying at 80 deg.C for 24 hr, and grinding to obtain HNTs-loaded molybdate and CaMoO4Encapsulated corrosion inhibitor material (Ca-Na)2MoO4-HNTs)。
Example 2
(1) Mixing Na2MoO4·2H2O (10.0g) was dissolved in 100ml of deionized water, and then 8g of HNTs were added thereto to form a suspension, referred to as A suspension.
(2) Suspension A was transferred to a 100ml beaker, which was then placed in a vacuum tank and evacuated to 1.325E3Pa using a vacuum pump and maintained at that pressure for 60min, and the system was then placed again at atmospheric pressure for 120min, which was referred to as completing the loading process. The above cycle was repeated and 6 loading experiments were completed.
(3) Centrifuging and washing the sample after 6 times of loading, and then re-dispersing the sample into 3.0 wt% of CaCl2Stirring in the solution for 15min, centrifuging, washing, drying at 40 deg.C for 24 hr, and grinding to obtain HNTs-loaded molybdate and CaMoO4Encapsulated corrosion inhibitor material (Ca-Na)2MoO4-HNTs)。
Example 3
(1) Mixing Na2MoO4·2H2O (15.0g) was dissolved in 100ml of deionized water, and 6g of HNTs were added thereto to form a suspension, referred to as A suspension.
(2) Suspension A was transferred to a 100ml beaker, which was then placed in a vacuum tank and evacuated to 1.325E3Pa using a vacuum pump and maintained at that pressure for 120min, and the system was then placed again at atmospheric pressure for 30min, which was referred to as completing the loading process. The above cycle was repeated and 2 loading experiments were completed.
(3) Centrifuging and washing the sample after three times of loading, and then re-dispersing the sample into 1.0 wt% of CaCl2Stirring in the solution for 5min, centrifuging, washing, drying at 60 deg.C for 24 hr, and grinding to obtain HNTs-loaded molybdate and CaMoO4Encapsulated corrosion inhibitor material (Ca-Na)2MoO4-HNTs)。
Example 4
(1) Mixing Na2MoO4·2H2O (5.0g) was dissolved in 100ml of deionized water, and 6g of HNTs were added thereto to form a suspension, referred to as A suspension.
(2) Suspension A was transferred to a 100ml beaker, which was then placed in a vacuum tank and evacuated to 1.325E3Pa using a vacuum pump and maintained at that pressure for 45min, and the system was then placed again at atmospheric pressure for 120min, which was referred to as completing the loading process. The above cycle was repeated and 4 loading experiments were completed.
(3) Centrifuging and washing the sample after three times of loading, and then re-dispersing the sample into 0.1 wt% of CaCl2Stirring the solution for 90min, centrifuging, washing, drying at 50 deg.C for 24h, and grinding to obtain HNTs-loaded molybdate and CaMoO4Encapsulated corrosion inhibitor material (Ca-Na)2MoO4-HNTs)。
As shown in FIG. 1, HNTs, Na2MoO4-HNTs and Ca-Na2MoO4TEM images of HNTs samples. FIG. 1a is a photograph of original HNTs, FIG. 1b is a photograph of Na-loaded HNTs2MoO4The subsequent photographs, FIG. 1c, are with CaCl2Pictures after the interaction. As can be seen in FIG. 1a, the original HNTs had a distinct hollow tubular structure with a tube length of 0.1-1.0 μm. From FIG. 1b it can be seen that the HNTs were filled with some substance, indicating Na2MoO4Successfully loaded into HNTs. As can be seen in FIG. 1c, there was some insoluble material at the port and surface of the tube, indicating that the port was indeed coated with CaMoO4And (6) covering. FIG. 2 shows HNTs, Na2MoO4HNTs and pure Na2MoO4XRD pattern of the crystal. For the XRD patterns of HNTs, the diffraction peaks at 2 θ ═ 12.1 °,20.0 ° and 24.6 ° were the same as the standard patterns of HNTs, indicating that the samples were HNTs. For Na2MoO4-HNTs, newly appearing diffraction peaks at 21.1 °,28.2 ° and 29.1 ° 2 θ, with pure Na2MoO4Consistent, the morphology, taken in conjunction with FIG. 1, shows Na2MoO4The molecules were successfully loaded into HNTs tubes. FIG. 3 is HNTs, pure CaMoO4And different concentrations of CaCl2Ca-Na obtained after solution treatment2MoO4XRD patterns of HNTs. For the XRD patterns of HNTs, the diffraction peaks at 2 θ ═ 12.1 °,20.0 ° and 24.6 ° were the same as the standard patterns of HNTs, indicating that the samples were HNTs. For pure CaMoO4Diffraction peaks at 18.66 °,28.75 °,31.28 °,34.30 °,47.10 °,49.30 °,54.12 ° and 58.07 ° 2 θ and CaMoO4The standard maps are consistent, and the sample is CaMoO4. For Ca-Na2MoO4The diffraction peak of-HNTs, 2 theta 28.75 DEG is observed in the XRD pattern, which is illustrated in Ca-Na2MoO4The surface of HNTs did form insoluble CaMoO4And (4) crystals.
Therefore, the technical scheme of the invention adopts HNTs, sodium molybdate and CaCl2Sequentially loading sodium molybdate into HNTs by a vacuum negative pressure method, and then forming insoluble CaMoO at the port of the HNTs4Encapsulation of HNTs with composites and CaMoO4The release speed of the loaded molybdate is controlled, and the specific experimental data is as follows:
(1) sustained release characteristics-Ca-Na encapsulating different Ca ion concentrations2MoO4-HNTs material (0.05g) was added to 100ml of distilled water, and 5ml of release medium was taken out while adding 5ml of distilled water thereto at a suitable time. The MoO was measured at different times on the release medium using a UV-2700 UV-visible spectrophotometer4 2-Concentration of (d), sorting the data to obtain MoO4 2-The test results are shown in fig. 4. As can be seen from FIG. 4, Na2MoO4The release time of HNTs can be maintained for 100 min. In Na2MoO4Surface introduction of insoluble CaMoO into HNTs4After complexing, Na2MoO4The release speed of the medicine is obviously slowed down, and the release time can be maintained to be more than 600 min. Further, MoO increased with the Ca ion concentration4 2-From Ca-Na2MoO4The release rate in HNTs was decreasing and at a release time of 100min, Na without Ca ion treatment2MoO4HNTs had been completely liberated and Ca-Na was treated for 0.1 wt.%, 0.3 wt.%, 1.0 wt.% and 3.0 wt.%2MoO4HNTs, in the sequence 76%, 71%, 56% and 42%.
(2) Good corrosion inhibition effect: to study Ca-Na2MoO4Long-acting protective Effect of HNTs, Ca-Na treated with 3.0 wt% Ca ion2MoO4-HNTs (0.2g) were added to 200ml of a 3.5 wt% NaCl aqueous solution and Q235 steel was soaked for 1h in a solution with a release time of 1h, 4h, 10h and 24 h. Then, a classical three-electrode system (area 1 cm) was used2The Q235 steel is used as a working electrode, the saturated calomel electrode is used as a reference electrode, the platinum sheet electrode is used as a counter electrode), and the Autolab 302 electrochemical workstation is used for processing the Q235 steel in 3.5 wt% of NaCl and 3.5% of NaCl + Ca-Na2MoO4The impedance of HNTs in solution at different release times was tested, as shown in FIG. 5. As seen from FIG. 5, the arc radius of the capacitive reactance of the Q235 steel in the 3.5% NaCl solution is small. Adding Ca-Na2MoO4The capacitive arc radius becomes larger after the HNTs material is added into the NaCl solution, and the radius becomes larger gradually along with the increase of the release time. The corrosion inhibition efficiency at different times calculated according to the polarization resistance is respectively 33.25%, 41.02%, 54.83% and 60.62% in sequence.
The adjustment of the preparation process parameters according to the content of the invention can realize Ca-Na2MoO4Preparation of HNTs and Performance substantially in accordance with the examples-Corrosion inhibitors of the invention in Slow-Release MoO4 2-The application comprises loading molybdate into HNTs, and utilizing MoO of halloysite pipe orifice4 2-Interaction with Ca ions forms insoluble CaMoO at the halloysite port4Complexing to achieve a slow rate of release of molybdate radicals within the halloysite tube.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (9)
1. A controlled-release halloysite-supported molybdate corrosion inhibitor is characterized in that molybdate is loaded inside halloysite, and MoO at the orifice of the halloysite is utilized4 2-Interaction with Ca ions forms insoluble CaMoO at the ports of halloysite4Composite to achieve mitigation of MoO in halloysite tubes4 2-The release rate of (c).
2. A preparation method of a controlled-release halloysite-supported molybdate corrosion inhibitor is characterized by comprising the following steps:
step 1, dispersing halloysite in an aqueous solution of molybdate to form a suspension, and loading the molybdate into the halloysite in a vacuum environment by using a negative pressure method;
step 2, dispersing the product prepared in the step 1 into an aqueous solution containing calcium ions, continuously dispersing, and utilizing MoO of a halloysite nozzle4 2-Interaction with Ca ions forms insoluble CaMoO at the ports of halloysite4And (c) a complex.
3. The method for preparing a controlled release halloysite-supported molybdate corrosion inhibitor according to claim 2, wherein in step 1, the molybdate is sodium molybdate, potassium molybdate or ammonium molybdate.
4. The method for preparing the controlled-release halloysite-supported molybdate corrosion inhibitor according to claim 2, wherein in the step 1, the mass ratio of molybdate to halloysite is (5-15): (2-8), preferably (8-15): (5-8).
5. The method for preparing the halloysite-supported molybdate corrosion inhibitor with the controllable release as claimed in claim 2, wherein in the step 1, the suspension is placed in a vacuum environment, the vacuum degree is 1000-2000 Pa, the vacuum degree is maintained for 30-120 min, the vacuum degree is maintained for 30-60 min, then the normal pressure is recovered, the loading process is completed once, and the loading process is repeated for 2-6 times, so that the loading of molybdate into the halloysite is completed.
6. The method for preparing the controlled-release halloysite-supported molybdate corrosion inhibitor according to claim 2, wherein in the step 2, the aqueous solution containing calcium ions is an aqueous solution of calcium chloride, and the mass percentage of the calcium chloride is 0.1-6.0 wt%, preferably 2-5 wt%.
7. The method for preparing a controlled release halloysite-supported molybdate corrosion inhibitor according to claim 2, wherein in step 2, ultrasound or stirring is used for continuous dispersion, and the ultrasound or stirring time is 1-30 min, preferably 10-30 min.
8. The method for preparing the controlled release halloysite-supported molybdate corrosion inhibitor according to claim 2, wherein in step 2, after dispersion is stopped, the mixture is centrifuged, washed, dried at 40-90 ℃ for 20-24 h, and then ground.
9. The slow release MoO of the corrosion inhibitor of claim 14 2-The method is characterized in that molybdate is loaded inside HNTs, and MoO of halloysite nozzle is utilized4 2-Interaction with Ca ions forms insoluble CaMoO at the halloysite port4Complexing to achieve a slow rate of release of molybdate radicals within the halloysite tube.
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Application publication date: 20191224 |