CN102140642A - Sustained-release type benzoic acid radical anion intercalation layered double hydroxides (LDHs) anti-corrosion material for carbon steel as well as preparation and application thereof - Google Patents
Sustained-release type benzoic acid radical anion intercalation layered double hydroxides (LDHs) anti-corrosion material for carbon steel as well as preparation and application thereof Download PDFInfo
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- CN102140642A CN102140642A CN 201110041730 CN201110041730A CN102140642A CN 102140642 A CN102140642 A CN 102140642A CN 201110041730 CN201110041730 CN 201110041730 CN 201110041730 A CN201110041730 A CN 201110041730A CN 102140642 A CN102140642 A CN 102140642A
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Abstract
The invention relates to a sustained-release anti-corrosion technology, particularly relates to a sustained-release type benzoic acid radical anion intercalation layered double hydroxides (LDHs) anti-corrosion material for carbon steel as well as a preparation and an application thereof. The chemical composition general formula of the anti-corrosion material is [M<2+>(1-x)M<3+>x(OH)2]x +(C6H5COO<->)x.nH2O, wherein M<2+> represents any one of divalent metal ions such as Mg<2+>, Zn<2+>, Ni<2+>, Fe<2+> and Mn<2+>; M<3+. represents any one of trivalent metal ions such as Al<3+>, Cr<3+>, Fe<3+>, V<3+>, Co<3+>, Ga<3+> and Ti<3+>; the molar ratio of M<2+> to M<3+> is 1.6-4.5, and x is less than or equal to 0.2 and more than or equal to 0.4. The material can be used as the anti-corrosion material in a neutral medium for carbon steel, and has potential application value in intelligent anti-corrosion coatings.
Description
Technical field
The present invention relates to the slowly-releasing aseptic technic, a kind of specifically slow release type benzoate anion anion intercalation hydrotalcite carbon steel anticorrosive and preparation and application.
Background technology
Corrosion is the material destruction of taking place under various environmental activities and rotten, spreads all over each department of national economy, brings massive losses to national economy.Protective coating is the most frequently used corrosion protection method.Traditional Chromium coating is widely used because of having the favorable protection effect.But, because chromic high toxicity is forbidden gradually.Therefore, the new environmentally friendly guard technology of exploitation is imperative.In recent years, the research of nanometer self-repair material becomes focus.As a kind of new function material, self-repair material is a kind of good intelligent material, can carry out self-recovery to subsurface defect, has broad prospect of application aspect metal anticorrosion.
(layered double hydroxides LDHs) is a kind of typical stratiform anionic clay to hydrotalcite, because it has good interlayer ion interchangeability, in recent years, hydrotalcite has caused people's extensive concern in the research of corrosion-resistant field.
Summary of the invention
The purpose of this invention is to provide a kind of slow release type benzoate anion anion intercalation hydrotalcite carbon steel anticorrosive and preparation and application.
For achieving the above object, the technical solution used in the present invention is:
A kind of slow release type benzoate anion anion intercalation hydrotalcite carbon steel anticorrosive: described anticorrosive chemical constitution general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
6H
5COO
-)
xNH
2O, M
2+Represent divalent-metal ion Mg
2+, Zn
2+, Ni
2+, Fe
2+, Mn
2+In any, M
3+Represent trivalent metal ion Al
3+, Cr
3+, Fe
3+, V
3+, Co
3+, Ga
3+, Ti
3+In any, M
2+/ M
3+Mol ratio be 1.6～4.5 (1.6,2.0,2.5,3,3.6,4,4.2 or 4.5); ≤ x≤0.4 0.2 (0.2,0.25,0.3,0.35 or 0.4).Described M
2+Divalent-metal ion is Mg
2+Described M
3+Trivalent metal ion is Al
3+
The preparation method of slow release type benzoate anion anion intercalation hydrotalcite carbon steel anticorrosive:
With M
2+Soluble salt and M
3+Soluble salt, press M
2+/ M
3+Mol ratio is that the ratio of 2-4 (2,2.5,3,3.5 or 4) is dissolved in and takes off CO
2Deionized water in be made into mixing salt solution, make M
2+Concentration be 0.10-1.60 (0.1,0.4,0.6,0.8,1.0,1.2,1.4 or 1.6) mol/L; NaOH is dissolved in takes off CO
2Deionized water in be mixed with the alkaline solution that concentration is 0.50-2.00 (0.5,0.7,0.8,0.9,1.2,1.4,1.6,1.8 or 2.0) mol/L; With above-mentioned two kinds of solution at N
2Protection is added dropwise to be dissolved in down simultaneously takes off CO
2The benzoic acid solution of deionized water, wherein benzoic mole number is M
2+And M
3+The 2-4 that mole number closes (2,2.2,2.4,2.6,2.8,3.0,3.2,3.4,3.6,3.8 or 4) times, keeping the pH value of system in the dropping process is 8-12 (8,9,10,11 or 12).With the slurries that obtain at N
2Protection under 40-100 (40,50,60,70,80,90 or 100) ℃ condition crystallization 2-24 (2,4,6,8,10,12,14,16,18,20,22 or 24) hour down is with taking off CO
2Deionized water wash, filter, with filter cake vacuum-drying 12-24 (12,14,16,18,20,22 or 24) h at room temperature, obtain phenylformic acid intercalated houghite precursor.
Described M
2+Represent divalent-metal ion Mg
2+, Zn
2+, Ni
2+, Fe
2+, Mn
2+In any, M
3+Represent trivalent metal ion Al
3+, Cr
3+, Fe
3+, V
3+, Co
3+, Ga
3+, Ti
3+In any; M
2+/ M
3+Mol ratio be 1.6～4.5 (1.6,2.0,2.5,3,3.6,4,4.2 or 4.5); ≤ x≤0.4 0.2 (0.2,0.25,0.3,0.35 or 0.4).
Described M
2+Divalent-metal ion is Mg
2+Described M
3+Trivalent metal ion is Al
3+Described solubility divalent metal salt can be any one in nitrate, chlorate or the vitriol, and the solubility trivalent metal salt can be any one in nitrate, chlorate or the vitriol.
The application of slow release type benzoate anion anion intercalation hydrotalcite carbon steel anticorrosive: described anticorrosive can be used as the anticorrosive of carbon steel in neutral medium.
Effect of the present invention and advantage are: the invention provides a kind of slow release type benzoate anion anion intercalation hydrotalcite impregnating material and preparation method thereof, this material is introduced hydrotalcite layers with the benzoate anion negatively charged ion, reach by corrosive ion in the corrosive environment and the anionic exchange of interlayer benzoate anion and to discharge benzoate anion negatively charged ion inhibiter, reach the purpose that to the carbon steel corrosion in neutral medium provides protection; Simultaneously, realized absorption, stopped its erosion, be expected to use the function that reaches the inhibition corrosion and repair matrix surface as the filler of intelligent erosion shield to the metallic surface to corrosive ion.
Description of drawings
The XRD spectra of the anion intercalated Zn-Al LDHs of gained benzoate anion (Zn/Al=2) that Fig. 1 provides for the embodiment of the invention (X-coordinate-angle 2 θ wherein, unit is ° (degree); Ordinate zou-intensity, unit is a.u. (absolute units)).
(X-coordinate-wave number, unit is nm to Fig. 2 for the FT-IR spectrogram of the anion intercalated Zn-Al LDHs of the gained benzoate anion that the embodiment of the invention provided (Zn/Al=2)
-1(every nanometer); Ordinate zou-intensity, unit is a.u. (absolute units)).
Fig. 3 is containing 50g L for the gained carbon steel electrode that the embodiment of the invention provided
-1The Ta Feier polarization curve of different time of releasing in the anion intercalated Zn-Al LDHs of benzoate anion (Zn/Al=2) the 3.5%NaCl solution (X-coordinate-electric current wherein, the mAcm of unit
-2(every square centimeter of milliampere); Ordinate zou-voltage, the V of unit (volt)).
Embodiment
Described anticorrosive chemical constitution general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
6H
5COO
-)
xNH
2O, M
2+Represent divalent-metal ion Zn
2+, M
3+Represent trivalent metal ion Al
3+M
2+/ M
3+Mol ratio be 2; X is 0.33.
Preparation process:
Experimental water eliminates CO for the secondary deionized water of just having boiled
2, be reflected at N
2Carry out under the atmosphere.Zn (NO
3)
26H
2O and Al (NO
3)
39H
2O is made into the mixing solutions (Zn of 1mol/L
2+/ Al
3+=2), be added drop-wise to (BZ/NO in Sodium Benzoate (BZ) solution
3 -=2).By dripping 1mol/LNaOH solution, vigorous stirring keeps pH=8 simultaneously.The gained slurries are 50 ℃ of crystallization 24h in encloses container.Cooling, washing, centrifugation, room temperature vacuum-drying 24h obtains the anion intercalated Zn-Al LDHs of benzoate anion (Zn/Al=2).XRD test shows product has good crystal formation, belongs to hexagonal system, the obvious (see figure 1) of laminate structure feature of LDH.FT-IR test shows benzoate anion is the unique object negatively charged ion (Fig. 2) of interlayer.
Carbon steel electrode as working electrode, is adopted
Epoxy encapsulation, electrodes exposed area 0.196cm
2, platinum wire electrode is a supporting electrode, and silver/silver chloride (Ag/AgCl, 3M KCl) electrode is a reference electrode, and ionogen is the 3.5%NaCl solution that contains 50g/L benzoate anion anion intercalation hydrotalcite of above-mentioned preparation, is assembled into three electrode test systems.Utilize the U.S. 760C of CHI company type electrochemical workstation to carry out the test of Ta Feier polarization curve, test potential is-300 to 300mV (vs.E
Oc) (E
OcBe open circuit potential), sweep velocity 0.5mV/s.In polarization method, equation 1 is used to calculate inhibition efficiency (η
p), i ' wherein
CorrAnd i
CorrBe respectively to have and do not have the current density of inhibiter under existing.
Ta Feier polarization curve test result shows to have good slowly-releasing antiseptic property by this material (wherein instrument uses the Japanese D/MAX of company of science 2500 type X-ray diffractometer (XRD) (Cu K
αRadiation,
) the sign product structure.Adopt the U.S.'s Nicolet iS of power ﹠ light company 10 Fourier transform infrared spectroscopy (FT-IR) to characterize interlayer object anion species.)。
Adding the Ta Feier polarization curve table with test results open fire talcum of benzoate anion intercalation Zn-Al LDHs (Zn/Al=2) when discharging different time in 3.5%NaCl solution can immobilized benzoate anion negatively charged ion and prolong and control its release rate, to reach the effect (Fig. 3) that suppresses corrosion of carbon steel in neutral medium.
Described anticorrosive chemical constitution general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
6H
5COO
-)
xNH
2O, M
2+Represent divalent-metal ion Mg
2+, M
3+Represent trivalent metal ion Al
3+M
2+/ M
3+Mol ratio be 3; X is 0.25.
Experimental water eliminates CO for the secondary deionized water of just having boiled
2, be reflected at N
2Carry out under the atmosphere.Mg (NO
3)
26H
2O and Al (NO
3)
39H
2O is made into the mixing solutions (Mg of 1mol/L
2+/ Al
3+=3), be added drop-wise to (BZ/NO in Sodium Benzoate (BZ) solution
3 -=4).By dripping 0.5mol/LNaOH solution, vigorous stirring keeps pH=10 simultaneously.The gained slurries are 80 ℃ of crystallization 6h in encloses container.Cooling, washing, centrifugation, room temperature vacuum-drying 24h obtains benzoate anion intercalation Mg-Al LDHs (Mg/Al=2).Ta Feier polarization curve test result shows that the corrosion in 3.5%NaCl solution has the good slow release protection effect to the anion intercalated Mg-AlLDHs of benzoate anion (Mg/Al=2) to carbon steel.
Described anticorrosive chemical constitution general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
6H
5COO
-)
xNH
2O, M
2+Represent divalent-metal ion Ni
2+, M
3+Represent trivalent metal ion Al
3+M
2+/ M
3+Mol ratio be 4; X is 0.20.
Experimental water eliminates CO for the secondary deionized water of just having boiled
2, be reflected at N
2Carry out under the atmosphere.Ni (NO
3)
26H
2O and Al (NO
3)
39H
2O is made into the mixing solutions (Ni of 1mol/L
2+/ Al
3+=4), be added drop-wise to (BZ/NO in Sodium Benzoate (BZ) solution
3 -=3).By dripping 1mol/LNaOH solution, vigorous stirring keeps pH=10 simultaneously.The gained slurries are 100 ℃ of crystallization 16h in encloses container.Cooling, washing, centrifugation, room temperature vacuum-drying 12h obtains the anion intercalated Ni-Al LDHs of benzoate anion (Ni/Al=4).Ta Feier polarization curve test result shows that the corrosion in 3.5%NaCl solution has the good slow release protection effect to benzoate anion intercalation Ni-AlLDHs (Ni/Al=4) to carbon steel.
Described anticorrosive chemical constitution general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
6H
5COO
-)
xNH
2O, M
2+Represent divalent-metal ion Mg
2+, Zn
2+, Ni
2+, Fe
2+, Mn
2+In any, M
3+Represent trivalent metal ion Al
3+, Cr
3+, Fe
3+, V
3+, Co
3+, Ga
3+, Ti
3+In any, M
2+/ M
3+Mol ratio be 1.6～4.5 (1.6,2.0,2.5,3,3.6,4,4.2 or 4.5); ≤ x≤0.4 0.2 (0.2,0.25,0.3,0.35 or 0.4).
Preparation process:
With M
2+Soluble salt and M
3+Soluble salt, press M
2+/ M
3+Mol ratio is that the ratio of 2～4 (2,2.5,3,3.5 or 4) is dissolved in and takes off CO
2Deionized water in be made into mixing salt solution, make M
2+Concentration be 0.10～1.60 (0.1,0.4,0.6,0.8,1.0,1.2,1.4 or 1.6) mol/L; NaOH is dissolved in takes off CO
2Deionized water in be mixed with the alkaline solution that concentration is 0.50～2.00 (0.5,0.7,0.8,0.9,1.2,1.4,1.6,1.8 or 2.0) mol/L; With above-mentioned two kinds of solution at N
2Protection is added dropwise to be dissolved in down simultaneously takes off CO
2The benzoic acid solution of deionized water, wherein benzoic mole number is M
2+And M
3+2～4 (2,2.2,2.4,2.6,2.8,3.0,3.2,3.4,3.6,3.8 or 4) that mole number closes doubly, keeping the pH value of system in the dropping process is 8～12 (8,9,10,11 or 12).With the slurries that obtain at N
2Protection is crystallization 2～24 (2,4,6,8,10,12,14,16,18,20,22 or 24) hour under 40～100 (40,50,60,70,80,90 or 100) ℃ condition down, with taking off CO
2Deionized water wash, filter, with filter cake vacuum-drying at room temperature 12～24 (12,14,16,18,20,22 or 24) h, obtain phenylformic acid intercalated houghite precursor.
Described solubility divalent metal salt can be any one in nitrate, chlorate or the vitriol, and the solubility trivalent metal salt can be any one in nitrate, chlorate or the vitriol.
Claims (9)
1. slow release type benzoate anion anion intercalation hydrotalcite carbon steel anticorrosive, it is characterized in that: described anticorrosive chemical constitution general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
6H
5COO
-)
xNH
2O, M
2+Represent divalent-metal ion Mg
2+, Zn
2+, Ni
2+, Fe
2+, Mn
2+In any, M
3+Represent trivalent metal ion Al
3+, Cr
3+, Fe
3+, V
3+, Co
3+, Ga
3+, Ti
3+In any; M
2+/ M
3+Mol ratio be 1.6～4.5; 0.2≤x≤0.4.
2. by the described slow release type benzoate anion of claim 1 anion intercalation hydrotalcite carbon steel anticorrosive, it is characterized in that: described M
2+Divalent-metal ion is Mg
2+
3. by the described slow release type benzoate anion of claim 1 anion intercalation hydrotalcite carbon steel anticorrosive, it is characterized in that: described M
3+Trivalent metal ion is Al
3+
4. the preparation method of the described slow release type benzoate anion of claim 1 an anion intercalation hydrotalcite carbon steel anticorrosive is characterized in that:
1) with M
2+Soluble salt and M
3+Soluble salt, press M
2+/ M
3+Mol ratio is that 2～4 ratio is dissolved in and takes off CO
2Deionized water in be made into mixing salt solution, make M
2+Concentration be 0.10～1.60mol/L, stand-by;
2) NaOH is dissolved in takes off CO
2Deionized water in be mixed with the alkaline solution that concentration is 0.50～2.00mol/L, stand-by;
3) with step 1) and step 2) above-mentioned two kinds of solution are at N
2Protection is added dropwise to be dissolved in down simultaneously takes off CO
2The Sodium Benzoate solution of deionized water, wherein the anionic mole number of benzoate anion is M
2+And M
3+2～4 times of closing of mole number, keeping the pH value of system in the dropping process is 8～12;
4) slurries that above-mentioned mixing is obtained are at N
2Protection is crystallization 2～24h under 40～100 ℃ of conditions down, with taking off CO
2Deionized water wash, filter, with filter cake vacuum-drying 12～24h at room temperature, obtain the benzoate anion anion intercalation hydrotalcite, the chemical constitution general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
6H
5COO
-)
xNH
2The carbon steel anticorrosive of O.
5. by the preparation method of the described slow release type benzoate anion of claim 4 anion intercalation hydrotalcite carbon steel anticorrosive, it is characterized in that: described M
2+Represent divalent-metal ion Mg
2+, Zn
2+, Ni
2+, Fe
2+, Mn
2+In any, M
3+Represent trivalent metal ion Al
3+, Cr
3+, Fe
3+, V
3+, Co
3+, Ga
3+, Ti
3+In any; M
2+/ M
3+Mol ratio be 1.6～4.5; 0.2≤x≤0.4.
6. by the preparation method of the described slow release type benzoate anion of claim 5 anion intercalation hydrotalcite carbon steel anticorrosive, it is characterized in that: described M
2+Divalent-metal ion is Mg
2+
7. by the preparation method of the described slow release type benzoate anion of claim 5 anion intercalation hydrotalcite carbon steel anticorrosive, it is characterized in that: described M
3+Trivalent metal ion is Al
3+
8. press the preparation method of the described slow release type benzoate anion of claim 5 anion intercalation hydrotalcite carbon steel anticorrosive, it is characterized in that: described solubility divalent metal salt can be any one in nitrate, chlorate or the vitriol, and the solubility trivalent metal salt can be any one in nitrate, chlorate or the vitriol.
9. the application of the described slow release type benzoate anion of claim 1 an anion intercalation hydrotalcite carbon steel anticorrosive, it is characterized in that: described anticorrosive can be used as the anticorrosive of carbon steel in neutral medium.
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| CN110724401A (en) * | 2019-11-22 | 2020-01-24 | 浙江丰虹新材料股份有限公司 | Synergistic self-repairing corrosion-resistant additive and application thereof |
| CN114364752A (en) * | 2019-11-22 | 2022-04-15 | 浙江丰虹新材料股份有限公司 | Synergistic self-repairing corrosion-resistant additive and application thereof |
| CN111039390A (en) * | 2019-12-26 | 2020-04-21 | 浙江伊诺环保科技股份有限公司 | Preparation method of microbial carbon source |
| CN111039390B (en) * | 2019-12-26 | 2022-05-17 | 浙江伊诺环保科技股份有限公司 | Preparation method of microbial carbon source |
| CN113564573A (en) * | 2021-07-22 | 2021-10-29 | 重庆大学 | Preparation method and application of magnesium alloy surface SLIPS/LDHs composite film layer |
| CN113598179A (en) * | 2021-09-07 | 2021-11-05 | 淄博职业学院 | Slow-release bactericide suitable for pet breeding environment and preparation method thereof |
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