CN108383408B - Calcium type zeolite-based imidazoline corrosion inhibitor and preparation method and application thereof - Google Patents

Calcium type zeolite-based imidazoline corrosion inhibitor and preparation method and application thereof Download PDF

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CN108383408B
CN108383408B CN201810210460.5A CN201810210460A CN108383408B CN 108383408 B CN108383408 B CN 108383408B CN 201810210460 A CN201810210460 A CN 201810210460A CN 108383408 B CN108383408 B CN 108383408B
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zeolite
type zeolite
corrosion inhibitor
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CN108383408A (en
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韦江雄
杨振国
胡捷
方圣雁
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South China University of Technology SCUT
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/60—Agents for protection against chemical, physical or biological attack
    • C04B2103/61—Corrosion inhibitors

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Abstract

The invention belongs to the technical field of preparation of reinforced concrete corrosion inhibitors, and particularly relates to a calcium type zeolite-based imidazoline corrosion inhibitor, and a preparation method and application thereof. In the method, firstly, pretreated zeolite is modified to obtain a calcium type zeolite carrier, and then imidazoline loading is carried out under the conditions of vacuum and normal temperature. The method is simple, takes the zeolite as a carrier, has wide material source and low cost, and the obtained corrosion inhibitor has good compatibility with a cement base. In addition, by modifying the zeolite, the pore volume of the obtained calcium-type zeolite can be increased by 80 percent compared with that of the pretreated zeolite, and the loading rate of imidazoline can be increased from 2 percent to 14 percent. The calcium type zeolite-based imidazoline corrosion inhibitor obtained by the method is used for reinforced concrete, can effectively avoid the defects of serious loss, short rust-resisting time and the like of the traditional internally-doped rust inhibitor, has no biotoxicity, and has wide application prospect.

Description

Calcium type zeolite-based imidazoline corrosion inhibitor and preparation method and application thereof
Technical Field
The invention belongs to the technical field of preparation of reinforced concrete corrosion inhibitors, and particularly relates to a calcium type zeolite-based imidazoline corrosion inhibitor, and a preparation method and application thereof.
Background
Reinforced concrete has become one of the most widely used building materials due to its advantages of low cost, firmness, durability, and wide material sources. However, the change of natural conditions such as wind, sunlight, rain and the like can cause the corrosion of the steel bars, which causes that a plurality of building structures have to be overhauled or rebuilt, thereby causing the service life to be limited. Especially for reinforced concrete building structures in ports or docks, the corrosion is more severe due to salt spray and chlorine ion invasion in seawater, and thus the design requirements are higher.
Aiming at the problem of steel bar corrosion, measures of 'prevention is mainly adopted and prevention and control are combined' are generally adopted at present, and specific methods for 'prevention' comprise cathode protection, surface coating or film coating, internal doping of a rust inhibitor and the like. The internally doped rust inhibitor is generally applied to the corrosion protection of steel bars with various structures due to the advantages of simple construction, low cost, good rust inhibition effect and the like. However, the internally doped rust inhibitor also has some disadvantages at present: (1) the effective rust-resisting time is short. (2) The rust inhibitor is dissolved out of the porous concrete along with natural factors such as wind, sunshine and the like and self change, so that the rust-proof performance of the reinforcing steel bar is reduced, and the environment is polluted.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention provides a preparation method of a calcium type zeolite-based imidazoline corrosion inhibitor.
Another object of the present invention is to provide a calcium-type zeolite-based imidazoline corrosion inhibitor prepared by the above method.
The invention also aims to provide application of the calcium type zeolite-based imidazoline corrosion inhibitor.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a calcium type zeolite-based imidazoline corrosion inhibitor comprises the following steps:
(1) preparation of calcium type zeolite carrier:
pretreating zeolite, reacting the pretreated zeolite with an acid solution and an alkali solution in sequence, centrifuging, washing and filtering in sequence until filtrate is neutral to obtain acid-base comprehensive modified zeolite, and reacting the acid-base comprehensive modified zeolite with a calcium salt solution to obtain a calcium type zeolite carrier;
(2) loading of imidazoline:
mixing the calcium type zeolite carrier and the imidazoline acetone solution, dipping under the conditions of vacuum, stirring and normal temperature, and then sequentially centrifuging, washing and drying the product to obtain the calcium type zeolite-based imidazoline corrosion inhibitor.
The imidazoline is prepared according to the synthesis and anti-corrosion performance of a cationic imidazoline rust inhibitor (J, 2012, 10(40)) of the balance of handsome and the like.
The invention takes zeolite as a carrier and loads imidazoline with good rust-resistant function, so that the obtained corrosion inhibitor has better compatibility with reinforced concrete. The calcium type zeolite carrier is obtained by modifying the zeolite, the loading rate of the zeolite to the imidazoline can be obviously improved, so that the corrosion resistance of the imidazoline to reinforced concrete can be fully exerted, and under the action of an external natural environment, the corrosion inhibitor is difficult to dissolve out and has long corrosion resistance time.
Preferably, the zeolite pretreatment method in the step (1) is specifically as follows: ball-milling zeolite to obtain zeolite powder with particle size less than 0.154mm, mixing the zeolite powder with deionized water at a solid-to-liquid ratio of 1:3g/ml, washing with water at 70 deg.C for 2 hr, and repeating the washing for several times until the supernatant is clarified after centrifugation.
More preferably, the particle size of the zeolite powder is 0.0385-0.074 mm.
Preferably, the solid-to-liquid ratio of the zeolite to the acid solution in the step (1) is 1:5 g/ml.
Preferably, the reaction time of the zeolite with the acid solution in step (1) is 2 h.
Preferably, the solid-to-liquid ratio of the zeolite to the alkali solution in the step (1) is 1:5 g/ml.
Preferably, the reaction time of the zeolite with the alkali solution in step (1) is 2 hours.
Preferably, the acid solution in step (1) is 1mol/L HCl.
Preferably, the alkali solution in the step (1) is 1mol/L NaOH.
Preferably, the calcium salt solution in step (1) is saturated CaCl2And (3) solution.
Preferably, the solid-to-liquid ratio of the acid-base comprehensive modified zeolite to the calcium salt solution in the step (1) is 1:5 g/ml.
Preferably, the reaction temperature of the acid-base comprehensive modified zeolite and the calcium salt solution in the step (1) is 80 ℃, and the reaction time is 4 hours.
Preferably, the concentration of the imidazoline acetone solution in the step (2) is 10 g/L.
Preferably, the solid-to-liquid ratio of the calcium-type zeolite carrier to the imidazolidinone acetone solution in the step (2) is 1:10 g/ml.
Preferably, the normal temperature in the step (2) is 20-40 ℃.
Preferably, the impregnation time in step (2) is 4 h.
Preferably, the drying temperature in step (2) is 60 ℃ and the time duration is 2 h.
The invention further provides a calcium type zeolite-based imidazoline corrosion inhibitor, which is prepared by the method.
The invention further provides an application of the calcium zeolite imidazoline corrosion inhibitor, and the corrosion inhibitor is used for corrosion prevention of reinforced concrete.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the calcium zeolite-based imidazoline corrosion inhibitor prepared by using zeolite as a carrier has the advantages of wide material source, low cost and simple preparation method. In addition, the zeolite carrier has the function of mineral admixture, so that the corrosion inhibitor has good compatibility with cement-based materials.
(2) The invention modifies zeolite, the pore volume of the obtained calcium zeolite can be improved by 80% compared with the initial pretreatment zeolite, and the loading rate of imidazoline can be improved to 14% from 2%.
(3) The calcium zeolite-based imidazoline corrosion inhibitor obtained by the invention is used for reinforced concrete, can effectively avoid the defects of serious loss, short rust resistance time and the like of the traditional internally doped rust inhibitor, and belongs to nondestructive repair. In addition, the corrosion inhibitor has no biological toxicity and is harmless to the environment, so the corrosion inhibitor has wide industrial application prospect.
Drawings
Fig. 1 is a pore structure distribution diagram of pretreated zeolite and calcium-type zeolite support prepared in example 1: FIG. 1 (A) is a graph showing cumulative pore volume distributions of pretreated zeolite and calcium-type zeolite carriers; fig. 1 (B) shows pore size distribution diagrams of the pretreated zeolite and the calcium-type zeolite support.
FIG. 2 is an infrared spectrum of the pretreated zeolite prepared in example 1 before and after loading imidazoline.
Fig. 3 is an infrared spectrum of three calcium-type zeolite carriers with different size fractions prepared in example 1 before and after loading imidazoline: FIG. 3 (A) is an infrared spectrum before and after imidazoline loading of a calcium zeolite carrier with a particle size of 0mm-0.0385 mm; FIG. 3 (B) is an infrared spectrum before and after imidazoline loading of the calcium zeolite carrier with a particle size of 0.0385mm-0.074 mm; FIG. 3 (C) is an infrared spectrum of the calcium type zeolite carrier having a particle size of 0.074mm to 0.154mm before and after loading imidazoline.
FIG. 4 is an infrared spectrum of imidazoline used in example 1.
FIG. 5 is a TG-DTG curve of imidazoline used in example 1.
Fig. 6 is a TG curve of the pretreated zeolite prepared in example 1 before and after loading the imidazoline.
Fig. 7 is a TG curve of the calcium-type zeolite prepared in example 1 before and after loading of imidazoline: FIG. 7 (A) is a TG curve before and after imidazoline loading of a calcium type zeolite carrier having a particle diameter of 0mm to 0.0385 mm; FIG. 7 (B) is a TG curve before and after loading imidazoline on a calcium type zeolite carrier having a particle diameter of 0.0385mm to 0.074 mm; FIG. 7 (C) is a TG curve before and after loading imidazoline on the calcium type zeolite carrier having a particle diameter of 0.074mm to 0.154 mm.
FIG. 8 is a potentiodynamic polarization curve of the reinforcing bar mortar after 135 days, which is doped with imidazoline corrosion inhibitor in the same proportion and calcium-type zeolite-based imidazoline corrosion inhibitor prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited to these examples. For process parameters not specifically noted, reference may be made to conventional techniques.
Example 1
Preparation of calcium type zeolite imidazoline corrosion inhibitor:
(1) preparation of pretreated zeolite:
ball-milling natural zeolite, sieving to obtain zeolite powder with particle size less than 0.154mm, mixing the zeolite powder with deionized water at a solid-to-liquid ratio of 1:3g/ml, washing with water at 70 deg.C for 2h, and repeating the washing for several times until the supernatant is clarified after centrifugation to obtain pretreated zeolite. And (3) further sieving the pretreated zeolite to obtain three kinds of zeolite powder with different size fractions of 0mm-0.0385mm, 0.0385mm-0.074mm and 0.074-0.154mm, respectively classifying the zeolite powder with the three size fractions into A, B, C groups, and respectively carrying out the following steps (2) - (4).
(2) Preparation of calcium type zeolite carrier:
mixing the pretreated zeolite and 1mol/L hydrochloric acid solution according to the solid-to-liquid ratio of 1:5g/ml, reacting for 2 hours, centrifuging, washing with deionized water, and performing suction filtration until no Cl is contained in the filtrate-And then, mixing the hydrochloric acid modified zeolite with 1mol/L NaOH solution according to the solid-to-liquid ratio of 1:5g/ml, reacting for 2 hours, then centrifuging, washing with deionized water, and performing suction filtration until the filtrate is neutral to obtain the acid-base comprehensive modified zeolite. Comprehensively modifying zeolite with saturated CaCl2Mixing the solution according to the solid-to-liquid ratio of 1:5g/ml, heating to 80 ℃, carrying out ion exchange for 4h, and drying to obtain the calcium type zeolite carrier.
(3) Imidazoline loading of calcium-type zeolites:
and (3) putting the calcium type zeolite carrier prepared in the step (2) into a closed container, vacuumizing by using a vacuum pump to ensure that the pressure of the closed container is stabilized at-0.1 Mp, slowly adding 10g/L of the imidazolidinone solution into the closed container through a feeding valve to be mixed with the calcium type zeolite carrier (the solid-liquid ratio of the calcium type zeolite carrier to the imidazolidinone solution is 1:5g/ml), opening the vacuum pump again, closing the vacuum pump after the pressure in the closed container is stabilized at-0.1 Mp, and opening a magnetic stirrer to react for 4 hours. After the reaction, the air inlet was slowly opened, and the pressure in the closed vessel was returned to normal pressure by an isobaric pressure reduction method (five steps, 0.02Mp pressure reduction each time, and 15min pressure maintenance each step). Finally, centrifuging, washing and drying for 2h at the temperature of 60 ℃ to obtain the calcium type zeolite-based imidazoline corrosion inhibitor.
(4) Imidazoline loading of pretreated zeolites:
and (3) replacing the calcium type zeolite carrier in the step (3) with the pretreated zeolite with the particle size of 0.0385mm-0.074mm prepared in the step (1), and repeating the step (3) to obtain the pretreated zeolite-based imidazoline corrosion inhibitor.
Zeolite, Ca-Zeolite (0mm-0.0385mm), Ca-Zeolite (0.0385mm-0.074mm) Ca-Zeolite (0.074mm-0.154mm) lines in FIG. 1 correspond to pore size distributions of 0.0385mm-0.074mm particle size pretreated Zeolite prepared in step (1) and A, B, C three groups of calcium type Zeolite supports prepared in step (2), respectively. Comparing spectral lines Zeolite and Ca-Zeolite (0.0385mm-0.074mm), it can be known that the pore volume of the calcium type Zeolite carrier obtained after modification is obviously increased by 80% compared with that of pretreated Zeolite, and particularly the pore structure of the calcium type Zeolite carrier is increased by 30-100 nm. In comparison with the spectral lines Ca-Zeolite (0mm-0.0385mm), Ca-Zeolite (0.0385mm-0.074mm) Ca-Zeolite (0.074mm-0.154mm), it is found that the pore volume of the calcium type Zeolite with the particle size of 0.0385mm-0.074mm is the largest among the calcium type zeolites with three particle sizes.
Fig. 2 is an infrared spectrum before and after imidazoline loading by the pretreated zeolite in the step (4), and fig. 3 is an infrared spectrum before and after imidazoline loading by A, B, C three groups of calcium type zeolite carriers in the step (3). FIG. 4 is the infrared spectrum of imidazoline used in this experiment, which shows that the characteristic peak appears at 2800-3000cm-1Location. Comparing fig. 2, fig. 3 and fig. 4, it can be known that after loading, the infrared spectra of both the pretreated zeolite and the calcium-type zeolite show characteristic absorption peaks of imidazoline, which indicates that imidazoline has been successfully loaded.
Calculation of imidazoline loading:
the loading capacity is calculated by adopting a weight loss method, namely, the difference value between the weight loss percentages of pretreated zeolite or calcium zeolite loaded with the imidazoline rust inhibitor is calculated according to TG curves measured before and after the pretreated zeolite or the calcium zeolite is loaded with the imidazoline rust inhibitor to serve as the loading capacity. Imidazoline thermally decomposes completely at 610 ℃ (see figure 5). Considering that zeolite contains adsorbed water and zeolite water, directly using the difference between the weight loss amounts at 610 ℃ as the loading amount may affect the accuracy of the calculation. Therefore, when calculating the load, the difference between the weight loss amounts of the imidazoline at the temperature of 200-610 ℃ before and after the load is calculated, and then the final load is calculated according to the percentage of the weight loss amount of the imidazoline at the temperature of 200-610 ℃ in the complete decomposition. The specific load calculation formula is as follows:
Figure BDA0001597056290000051
wherein: q represents the load amount; k1 represents the weight loss percentage of imidazoline at the complete decomposition temperature of 200 ℃ and 610 ℃; k2 represents the weight loss percentage in the range of 200-610 ℃ before loading the pretreated zeolite or calcium-type zeolite; k3 represents the percent weight loss after loading of the pretreated zeolite or calcium-type zeolite in the range of 200 ℃ and 610 ℃.
As can be seen from fig. 5, the weight loss percentage of imidazoline at 610 ℃ of 200-1＝2.14％。
The weight loss percentages of the calcium type zeolite carriers with different particle sizes before and after loading imidazoline in the step (2) are respectively as follows: the weight loss percentages before and after loading of the calcium-type zeolite having a particle diameter of 0mm to 0.0385mm were 3.67% for K2 and 10.68% for K3 (see (a) in fig. 7), from which the loading amount of the calcium-type zeolite carrier was calculated as Q27.37%; the weight loss percentages before and after loading of the calcium-type zeolite having a particle size of 0.0385mm to 0.074mm were K2 ═ 4.24% and K3 ═ 17.52% (see (B) in fig. 7), and from this, the loading of the calcium-type zeolite carrier was calculated to be Q314.03%; the weight loss percentages before and after loading of the calcium-type zeolite having a particle size of 0.074mm to 0.154mm were 1.99% K2 and 13.60% K3 (see fig. 7 (C)), and from this, the loading of the calcium-type zeolite carrier was calculated as Q4＝12.26％
Comparison Q1、Q2、Q3、Q4It can be known that the calcium type zeolite carrier obtained after modification has higher imidazoline loading than the pretreated zeolite. Wherein the calcium type zeolite with the grain diameter of 0.0385mm-0.074mm has the best loading effect.
Example 2
The long-term rust inhibition effect experiment of the calcium type zeolite-based imidazoline slow release agent comprises the following steps:
the steel bar mortar is divided into two groups which are the same, and imidazoline corrosion inhibitors with the same proportion and the calcium type zeolite-based imidazoline corrosion inhibitor (with the grain diameter of 0.074mm-0.154mm) prepared in the example 1 are respectively doped. Wherein the water-cement ratio of the mortar is 0.5, the cement-sand ratio is 1:3, and the stirring is carried out according to GB/T17671-1999. The stirred mortar is added into a 40mm multiplied by 160mm grinding tool for fixing the reinforcing steel bars and is vibrated to be compact. Placing the formed sample in a standard constant temperature and humidity curing box (the relative humidity is 98 percent, the temperature is 20 ℃) for curing for 24 hours, then removing the mold, curing for 28 days under the condition that the temperature is 20 ℃ and the relative humidity is more than or equal to 95 percent to obtain two groups of reinforced mortar samples, respectively soaking the two groups of reinforced mortar samples in NaCl solution with the mass fraction of 3.5 percent, and performing electrochemical impedance spectroscopy and potentiodynamic polarization curve tests on the reinforced mortar soaked in the NaCl solution for a certain time by adopting an electrochemical workstation to represent the quality of the rust resistance effect.
FIG. 8 is a potentiodynamic polarization curve of the reinforcing bar mortar after 135 days, which is doped with imidazoline corrosion inhibitor in the same proportion and calcium-type zeolite-based imidazoline corrosion inhibitor prepared in example 1. The corrosion potential of the steel bar mortar doped with the calcium type zeolite-based imidazoline corrosion inhibitor is obviously greater than that of a corrosion inhibition sample directly doped with imidazoline, the corrosion current density is smaller, and the corrosion resistance effect is better as the corrosion potential is higher and the corrosion current density is lower, so that the calcium type zeolite-based imidazoline corrosion inhibitor has a better long-term corrosion resistance effect than the corrosion inhibitor directly doped with imidazoline.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. A preparation method of a calcium type zeolite-based imidazoline corrosion inhibitor for corrosion prevention of reinforced concrete is characterized by comprising the following steps:
(1) preparation of calcium type zeolite carrier:
pretreating zeolite, reacting the pretreated zeolite with an acid solution and an alkali solution in sequence, centrifuging, washing and filtering in sequence until filtrate is neutral to obtain acid-base comprehensive modified zeolite, and reacting the acid-base comprehensive modified zeolite with a calcium salt solution to obtain a calcium type zeolite carrier;
(2) loading of imidazoline:
mixing the calcium type zeolite carrier and the imidazoline acetone solution, dipping under the conditions of vacuum, stirring and normal temperature, and then sequentially centrifuging, washing and drying the product to obtain the calcium type zeolite-based imidazoline corrosion inhibitor.
2. The preparation method of the calcium type zeolite-based imidazoline corrosion inhibitor as claimed in claim 1, wherein the pretreatment method of the zeolite in the step (1) is specifically as follows: ball-milling zeolite to obtain zeolite powder with particle size less than 0.154mm, mixing the zeolite powder with deionized water at a solid-to-liquid ratio of 1:3g/ml, washing with water at 70 deg.C for 2 hr, and repeating the washing for several times until the supernatant is clarified after centrifugation.
3. The method for preparing the calcium type zeolite-based imidazoline corrosion inhibitor of claim 2, wherein the method comprises the following steps: the particle size of the zeolite powder is 0.0385-0.074 mm.
4. The method for preparing the calcium type zeolite-based imidazoline corrosion inhibitor of claim 1, wherein the method comprises the following steps: the calcium salt solution in the step (1) is saturated CaCl2And (3) solution.
5. The method for preparing the calcium type zeolite-based imidazoline corrosion inhibitor of claim 1, wherein the method comprises the following steps:
the concentration of the imidazoline acetone solution in the step (2) is 10 g/L;
and (3) the solid-to-liquid ratio of the calcium type zeolite carrier to the imidazoline acetone solution in the step (2) is 1:10 g/ml.
6. The method for preparing the calcium type zeolite-based imidazoline corrosion inhibitor of claim 1, wherein the method comprises the following steps: the reaction temperature of the acid-base comprehensive modified zeolite and the calcium salt solution in the step (1) is 80 ℃.
7. The method for preparing the calcium type zeolite-based imidazoline corrosion inhibitor of claim 1, wherein the method comprises the following steps: the solid-to-liquid ratio of the acid-base comprehensive modified zeolite to the calcium salt solution in the step (1) is 1:5 g/ml.
8. The method for preparing the calcium type zeolite-based imidazoline corrosion inhibitor of claim 1, wherein the method comprises the following steps:
the solid-to-liquid ratio of the zeolite to the acid solution in the step (1) is 1:5 g/ml;
the solid-to-liquid ratio of the zeolite to the alkali solution in the step (1) is 1:5 g/ml;
the acid solution in the step (1) is 1mol/L HCl;
the alkali solution in the step (1) is 1mol/L NaOH.
9. A calcium type zeolite-based imidazoline corrosion inhibitor is characterized in that: the calcium type zeolite-based imidazoline corrosion inhibitor is prepared by the method of any one of claims 1 to 8.
10. The use of the calcium type zeolite-based imidazoline corrosion inhibitor of claim 9, wherein: the calcium type zeolite-based imidazoline corrosion inhibitor is used for corrosion prevention of reinforced concrete.
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CN112679749B (en) * 2020-12-24 2022-03-29 华南理工大学 Zeolite-like zinc-based imidazole ester metal organic framework reinforcing steel bar corrosion inhibitor and preparation method and application thereof
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