CN101838120A - Migration-type organic reinforced concrete anti-corrosion admixture - Google Patents
Migration-type organic reinforced concrete anti-corrosion admixture Download PDFInfo
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- CN101838120A CN101838120A CN201010140907A CN201010140907A CN101838120A CN 101838120 A CN101838120 A CN 101838120A CN 201010140907 A CN201010140907 A CN 201010140907A CN 201010140907 A CN201010140907 A CN 201010140907A CN 101838120 A CN101838120 A CN 101838120A
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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
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/10—Compositions or ingredients thereof characterised by the absence or the very low content of a specific material
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/10—Compositions or ingredients thereof characterised by the absence or the very low content of a specific material
- C04B2111/1025—Alkali-free or very low alkali-content materials
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/26—Corrosion of reinforcement resistance
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Abstract
The invention relates to a migration-type organic reinforced concrete anti-corrosion admixture which is prepared by mixing organic carboxylic acid and organic amine in the following percentage by weight: 40-80% of the organic carboxylic acid and 20-60% of the organic amine; adding the mixture into water; heating to 60-70 DEG C; and stirring the mixture for reaction for 1-2 hours to obtain the migration-type organic reinforced concrete anti-corrosion admixture. The anti-corrosion admixture does not contain nitrite and inorganic base and can prevent damage on reinforcing steel bar passive films caused by chloride ions, thus preventing corrosion.
Description
Technical field
The present invention relates to a migration-type organic reinforced concrete anti-corrosion admixture, belong to technical field of concrete additives.
Background technology
Concrete is a kind of overbasic material, and under the normal circumstances, its high basicity must make rebar surface wherein form fine and close passive film, is the natural protective membrane of reinforcing bar.Yet the intrusion of carbonization of concrete and chlorion can destroy the passive state of reinforcing bar, causes its corrosion.Especially under water, over strait and western saline and alkaline geographic engineering, the danger of steel bar corrosion is then more serious.Have the expert to point out, steel bar corrosion is the destroying concrete structure most important reason.
From eighties of last century mid-term, people have just begun to pay close attention to the anticorrosion of reinforcing bar in the concrete, top coat, galvanic protection, electrochemical desalting and use rust inhibitor etc. all by in various degree application.But except that rust inhibitor, additive method all needs comparatively complicated operations, and cost is higher.That rust inhibitor is considered to is most economical, the resistance of most convenient rust approach.
Chemical compound lot all once was used to antirust for reinforced concrete, comprising: nitrite, dichromate, tin protochloride, hexahydroaniline, dicyclohexyl amine, sodium monoflurophosphate or the like.But they have separately comparatively significant disadvantages.
US3210207,3801338,4365999 etc. recommends calcium nitrite as the skeleton construction rust inhibitor.But, and the operator in the construction process are brought injury owing to it has tangible carinogenicity, can pollute environment.And when using quantity not sufficient, not only can not stop corrosion to take place, can quicken spot corrosion on the contrary.
CN101407385A has reported a kind of concrete steel bar rust inhibitor of alkali-free non-nitrous salt, is dissolved in water by Zinc Gluconate, lithium silicate, ammonium benzoate and lower molecular weight (alcohol) amine to make.Although wherein do not contain nitrite, it may affect greatly concrete performance, and major part remains inorganic salts, does not have good transfer ability.EP0787697A1 has reported that also the aqueous solution of glucoheptonic acid and molybdic acid an alkali metal salt is used for skeleton construction resistance rust.
CN1872770A has then used a spot of Sodium orthomolybdate, diethylenetriamine, propenyl thiocarbamide and the 1.4-butynediol antirust for reinforced concrete that makes a kind of low toxicity soluble in water, plays the effect that resistance is become rusty by the chemical reaction and the absorption of above-mentioned substance and reinforcing bar.But there are some researches show that the adsorption between micromolecular amine, alcohols and reinforcing bar is all less, enough infirm.US4276914 also once did the report that pure amine mixt is used for the concrete structure steel bar anti-corrosion.
US5916483 is spiked into the reaction product mixture of organic or inorganic acid with amine in the inorganic coagulation material, is used for the anticorrosion of material of construction reinforcing bar.And point out: this product without any unpleasant odor and the engineering health of operators is safe from harm.But the part that wherein plays the effect of resistance rust still is small molecule amine mostly, and its long-term effect that hinders rust in concrete remains further to be studied.
The material (as N, N-dimethylethanolamine, ammonium benzoate etc.) that US6174461B1, US6342101B1 then will have resistance rust effect respectively is spiked into concrete admixtures such as sealing agent, water reducer, use composite with it, thus play the effect that resistance is become rusty.
In sum, present antirust for reinforced concrete has been expanded to inorganic salt such as low toxicity or nontoxic molybdate, sodium monoflurophosphate by traditional nitrite, arrive neutralized reaction product of organic class thanomin, amine and acid or the like again.Inorganic salts mostly is anode type rust inhibitor, only just can show resistance rust effect preferably after consumption reaches certain value.As, there are some researches show: when nitrite used as reinforcing bar rust inhibitor in the bar in chlorine salt solution, the mol ratio of nitrite anions and chlorion＞1 o'clock could guarantee to have the good resistance effect of becoming rusty, if the content of nitrite is low excessively, not only do not have resistance rust effect, may quicken the corrosion of reinforcing bar on the contrary.Simultaneously, the inorganic salt too high alkali content that may bring also may cause the generation of harm such as concrete alkali aggregate reaction.In addition, such rust inhibitor has environmental pollution mostly, and a large amount of uses works the mischief for society and environment.The small-molecule substance that existing organic class rust inhibitor then is alcamines mostly simply mixes, composite use.But the common rate of diffusion of such rust inhibitor is very fast, thereby the long-term behaviour that causes hindering rust can not get guaranteeing.Simultaneously, find also in the practice that alcamines is micromolecular to add workability and the later stage mechanical property that affiliation influences the concrete mix.
Summary of the invention
The purpose of this invention is to provide a kind of migration-type organic reinforced concrete anti-corrosion admixture that does not contain nitrite, mineral alkali.This rust inhibitor can prevent the destruction of the rebar passivation film that chlorion causes, thereby prevents that corrosion from taking place.
The applicant is through discovering, good organic rust inhibitor can with the firm absorption of rebar surface, and its non-polar group arranges at rebar surface, forms hydrophobic layer, hinders contacting of harmful ions such as oxygen, OH-and reinforcing bar, thereby plays the protection action of steel bars.On the other hand, the rust inhibitor molecule is the process of absorption and desorption running balance in the covering of rebar surface.The rust inhibitor molecule is big more in the adsorptive capacity of rebar surface, and then coverage is big more, and resistance rust efficient must be high more.Thereby, the multiple molecule of different scale, different structure should be arranged in the rust inhibitor, complimentary to one another, fill, just can make adsorption layer finer and close.On the other hand, according to the Lewis acid-base theory, the easy and soft base coordination of soft acid, and hard acid is preferential and the hard base coordination.At rebar surface, zone of oxidation belongs to hard acid, the simple substance attitude is a soft acid.Thereby, to have hard base and soft base part in the rust inhibitor molecular structure simultaneously and just can better adsorb at rebar surface.
Based on above-mentioned research, the present invention proposes a kind of new migration-type organic reinforced concrete anti-corrosion admixture, and this rust inhibitor adopts following method preparation:
After organic carboxyl acid and amine mixed by following weight ratio, add in the entry, be heated to 60～70 ℃, stir, reaction is prepared from after 1～2 hour:
Above-mentioned organic carboxyl acid is selected from any one in following two groups of organic carboxyl acids:
The 1st group: lactic acid, gluconic acid, vinylformic acid, methacrylic acid;
The 2nd group: propionic acid, sad, lauric acid, phenylformic acid, tolyl acid, benzaminic acid, ethylenediamine tetraacetic acid (EDTA);
Or two or more in two or more and the 2nd group of organic carboxyl acid in above the 1st group of organic carboxyl acid by the use that is mixed of following weight ratio:
The 1st group of organic carboxyl acid: the 0～40%, 2nd group of organic carboxyl acid 60%～100%.
Above-mentioned organic amine is selected from any one of following two groups of organic amines:
The 1st group: thanomin, diethanolamine, trolamine, hexahydroaniline, dicyclohexyl amine, N, N-dimethylcyclohexylamine;
The 2nd group: N, N-dimethylethanolamine, N, N-diethylethanolamine, N, N-diethylpropanolamine, diisopropanolamine (DIPA), diethylenetriamine, triethylene tetramine, vulkacit H;
Or two or more in two or more and the 2nd group of organic amine in the 1st group of organic amine by the use that is mixed of following weight ratio:
The 1st group of organic amine: the 0～50%, 2nd group of organic amine: 50%～100%.
PH value of the present invention is between 7～9.
Rust inhibitor of the present invention is a kind of by organic carboxyl acid and the organic amine soluble carboxylic acid amine salt that the back generates that reacts, can be by shown in the following general formula:
Wherein, R may contain alkyl, phenyl and groups such as derivative, alkylene thereof, R
I, R
II, R
III, R
IVThen may be groups such as hydrogen, hydroxyl, cycloalkyl, amide group and alkanamine chain.Add C, N isopolarity atom in carboxyl, the amido, make and contain a plurality of polar functionalities groups in the rust inhibitor molecule of the present invention, when combining with the Fe atom, can form the chelate ring of 5 yuan or 6 yuan, the rust inhibitor of simple function groups such as its bonding force and stability and micromolecular hydramine is compared and is increased dramatically.In addition, the sub-ability of the power supply that has further increased them that combines of non-polar groups such as alkyl, cycloalkyl and polar group, thereby make the rust inhibitor molecule and combine more firmly with reinforcing bar, the rebar surface fraction of coverage increases, resistance rust effect improves thereupon.On the other hand, non-polar groups such as the alkyl in the rust inhibitor molecule, cycloalkyl are arranged at rebar surface, form hydrophobic layer, isolate harmful ion, protection action of steel bars thereby reach.The interactive molecular structure of this polyfunctional group has the incomparable advantage of unit molecule Compositional type rust inhibitor aspect the reinforcing bar binding ability.
Rust inhibitor of the present invention is the aqueous solution of stable homogeneous, so preparation process is carried out in water.Because water does not participate in reaction, so the consumption of water do not exert an influence to reaction result, just the concentration to the finished product rust inhibitor exerts an influence, and the consumption of the present invention when concrete the application exerted an influence.
The present invention can newly mix admixture in the process at concrete, plays the effect that stops Rust of Rebar in Concrete.Perhaps the present invention directly is coated in existing concrete structural surface,, can reaches the purpose of reinforcing bar in the protection structure by migration then by the adequate measure sealing.
The present invention has following advantage:
1, do not contain nitrite, can avoid the pollution of using nitrite environment to be brought in a large number as rust inhibitor;
2, compound rust inhibitor can be protected negative electrode and anode in the reinforcing bar electrochemical reaction simultaneously; The acceleration corrosion that does not exist similar inorganic salts rust inhibitor with quantity not sufficient the time, may cause; To structural safety;
3, anticorrosion performance efficiently has multiple functional group in the rust inhibitor molecule, can form the multicomponent chelate ring when combining with reinforcing bar, and combination stability significantly improves, and anticorrosion performance is particularly superior.This is the significant difference part of organic rust inhibitor of itself and one-component or the simple composite gained of organism small molecules;
4, the carboxylic acid in the rust inhibitor molecule runs into the Ca in the concrete
2+Can precipitate, may stop up the interior pore of concrete, stop the migration of objectionable impurities to a certain extent to its inside, can further prevent the generation of steel bar corrosion on the angle of protective layer.
5, rust inhibitor of the present invention and cement and other concrete admixtures have excellent adaptability.
Description of drawings
Fig. 1 (a) is reinforcing bar electrode electrochemical impedance spectroscopy Nyquist figure in containing the simulation solution of embodiment 1.
Fig. 1 (b) is reinforcing bar electrode electrochemical impedance spectroscopy Bode phase angle figure in containing the simulation solution of embodiment 1.
Fig. 2 (a) is reinforcing bar electrode electrochemical impedance spectroscopy Nyquist figure in containing the simulation solution of embodiment 2.
Fig. 2 (b) is reinforcing bar electrode electrochemical impedance spectroscopy Bode phase angle figure in containing the simulation solution of embodiment 2.
Fig. 3 (a) is reinforcing bar electrode electrochemical impedance spectroscopy Nyquist figure in containing the simulation solution of embodiment 3.
Fig. 3 (b) is reinforcing bar electrode electrochemical impedance spectroscopy Bode phase angle figure in containing the simulation solution of embodiment 3.
Fig. 4 (a) is reinforcing bar electrode electrochemical impedance spectroscopy Nyquist figure in containing the simulation solution of embodiment 4.
Fig. 4 (b) is reinforcing bar electrode electrochemical impedance spectroscopy Bode phase angle figure in containing the simulation solution of embodiment 4.
Fig. 5 (a) is reinforcing bar electrode electrochemical impedance spectroscopy Nyquist figure in containing the simulation solution of embodiment 5.
Fig. 5 (b) is reinforcing bar electrode electrochemical impedance spectroscopy Bode phase angle figure in containing the simulation solution of embodiment 5.
Fig. 6 is electrode equivalent electrical circuit in the simulation concrete hole solution of no rust inhibitor;
Fig. 7 contains electrode equivalent electrical circuit in the simulation concrete hole solution of rust inhibitor of the present invention.
Embodiment
With the reactant weight ratio is that propionic acid 41%, diethanolamine 59% mix, and adds the water identical with the reaction product total amount, is heated to 60 ℃, and stirring reaction 1 hour makes the antirust for reinforced concrete aqueous solution.Experimentize the result of gained such as Fig. 1 according to the aftermentioned experimental technique.
With the reactant weight ratio is phenylformic acid 58%, hexahydroaniline 13%, N, and N-dimethylethanolamine 29% mixes, and adds the water identical with the reaction product total amount, is heated to 60 ℃, and stirring reaction 1 hour makes the antirust for reinforced concrete aqueous solution.Experimentize the result of gained such as Fig. 2 according to the aftermentioned experimental technique.
With the reactant weight ratio is that sad 34%, o-toluic acid 31%, diisopropanolamine (DIPA) 25%, diethylenetriamine 10% mix, and adds the water identical with the reaction product total amount, is heated to 60 ℃, and stirring reaction 2 hours makes the antirust for reinforced concrete aqueous solution.Experimentize the result of gained such as Fig. 3 according to the aftermentioned experimental technique.
With the reactant weight ratio is 2-benzaminic acid 72%, gluconic acid 4%, diethylenetriamine 16%, trolamine 8% mixing, add the water identical with the reaction product total amount, be heated to 70 ℃, stirring reaction 1.5 hours makes the antirust for reinforced concrete aqueous solution.Experimentize the result of gained such as Fig. 4 according to the aftermentioned experimental technique.
With the reactant weight ratio is ethylenediamine tetraacetic acid (EDTA) 73%, diethylenetriamine 23%, trolamine 4%, adds the water identical with the reaction product total amount, is heated to 70 ℃, and hybrid reaction 1.5 hours makes the antirust for reinforced concrete aqueous solution.According to the resistance rust effect of above-mentioned testing method test rust inhibitor, result such as Fig. 5.
Experimental technique: in order to check the resistance rust effect of the rust inhibitor that this experiment makes, the present invention has adopted linear polarization and electrochemical impedance spectral method to test and estimate.Test is carried out on three-electrode system, and saturated calomel electrode is a reference electrode, and Pt is a supporting electrode.Utilize PAR 273A potentiostat to carry out the polarization curve test, sweep velocity is 1mV/s in the polarization curve.Utilize 273A potentiostat and 5210 lock-in amplifiers to carry out the test of electrochemical impedance spectroscopy, the survey frequency scope is 100KHz～10mHz, and ac-excited signal is 10mV.
Cylindrical reinforcing bar electrode with the Q235 plain bar processes is of a size of Φ 1.12cm * 1cm.With one of them end face is working face, draws the copper conductor of sealing from the other end welding.Put it in the pvc pipe that diameter is 2cm, and inject epoxy resin glue, make both tight bond to both spaces.The test before the reinforcing bar electrode polish step by step with the silicon carbide paper of 100～1000# successively, go dried up in ultrasonic cleaning.With the careful wiping working face of alcohol, remove the impurity such as grease on it before the test.
Simulation concrete hole liquid is 0.6mol/L KOH+0.2mol/L NaOH, uses NaHCO
3Solution is regulated about its pH value to 12.0, provides bar in chlorine salt solution to wherein adding the NaCl of massfraction for 3.5% then.The rust inhibitor of embodiment preparation is dissolved in the simulated solution, and the rust inhibitor mass concentration is 3%.After stirring the reinforcing bar electrode is soaked wherein, test the electrochemical impedance spectroscopy after 1 day.
According to JT/T 537-2004 " antirust for reinforced concrete " concrete performance after adding rust inhibitor of the present invention is tested.
Select suitable equivalent electrical circuit that the electrochemical impedance spectroscopy data shown in Fig. 1～Fig. 5 are carried out match, utilize the gained result to calculate the inhibition efficiency of rust inhibitor among the embodiment, as table 1.Since different when not containing in the simulated solution of rust inhibitor electrode state of living in and containing rust inhibitor, thereby its corresponding equivalent electrical circuit is also inequality, respectively as shown in Fig. 6, Fig. 7.Wherein, R
sThe expression solution resistance, R
cAnd C
cResistance and the electric capacity of representing rebar surface rust inhibitor layer or electrode surface chemical reaction product respectively, R
CtBe the charge transfer resistance of corrosion reaction, Q
CtBe the normal phase angle element of reinforcing bar interfacial electric double layer, W is the Warburg impedance.Wherein normal phase angle element Q
CtUse Y
0ctAnd n
CtCharacterize Warburg impedance Y
0wCharacterize.Permanent phase angle element Q can be expressed as Z
CPE=(j ω)
-n/ Y
0, Y in the formula
0Be called basic admittance, unit is Ω
-1, the span of n is 0＜n＜1, expression solid electrode electrostatic double layer departs from the degree of ideal capacitance.
Resistance rust efficient (IE) in the table 1 is basis
Calculate and come.R
CtBe the charge transfer resistance of electrode in the blank solution, R
Ct' for containing the charge transfer resistance of electrode in the simulated solution of inhibiter.
The resistance rust effect of table 1 rust inhibitor of the present invention
Antirust for reinforced concrete can not have a negative impact to the performance of concrete own when having good resistance rust effect.In embodiments of the present invention, carried out the test of concrete performance.Test index mainly comprises time of coagulation and ultimate compression strength, and the gained result is as shown in table 2.
Table 2 concrete technical feature
Annotate: this tests used cement is little wild field P.II 42.5R cement
The present invention can comprise that other does not depart from the specific form of the present invention's spirit or its essential characteristic.Therefore, Chan Shi embodiment only is used for explanation herein, is not construed as limiting the invention.Protection scope of the present invention should be with being as the criterion that the claim protection domain is defined.
Claims (4)
1. migration-type organic reinforced concrete anti-corrosion admixture is characterized in that organic carboxyl acid and organic amine are mixed by following weight ratio, adds in the entry, is heated to 60～70 ℃, and stirring, reaction were prepared from after 1～2 hour:
Organic carboxyl acid 40%～80%, organic amine 20%～60%.
2. migration-type organic reinforced concrete anti-corrosion admixture according to claim 1 is characterized in that described organic carboxyl acid is selected from any one in following two groups of organic carboxyl acids:
The 1st group: lactic acid, gluconic acid, vinylformic acid, methacrylic acid;
The 2nd group: propionic acid, sad, lauric acid, phenylformic acid, tolyl acid, benzaminic acid, ethylenediamine tetraacetic acid (EDTA);
Or two or more in two or more and the 2nd group of organic carboxyl acid in above the 1st group of organic carboxyl acid by the use that is mixed of following weight ratio:
The 1st group of organic carboxyl acid: the 0～40%, 2nd group of organic carboxyl acid 60%～100%.
3. migration-type organic reinforced concrete anti-corrosion admixture according to claim 1 is characterized in that described organic amine is selected from any one of following two groups of organic amines:
The 1st group: thanomin, diethanolamine, trolamine, hexahydroaniline, dicyclohexyl amine, N, N-dimethylcyclohexylamine;
The 2nd group: N, N-dimethylethanolamine, N, N-diethylethanolamine, N, N-diethylpropanolamine, diisopropanolamine (DIPA), diethylenetriamine, triethylene tetramine, vulkacit H;
Or two or more in two or more and the 2nd group of organic amine in the 1st group of organic amine by the use that is mixed of following weight ratio:
The 1st group of organic amine: the 0～50%, 2nd group of organic amine: 50%～100%.
4. as migration-type organic reinforced concrete anti-corrosion admixture as described in claim 1 or 2 or 3, it is characterized in that its pH value is between 7～9.
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| CN102584077A (en) * | 2012-01-16 | 2012-07-18 | 中国建筑科学研究院 | Loading-type reinforcing steel bar corrosion inhibitor and preparation method thereof |
| CN102775087A (en) * | 2012-08-07 | 2012-11-14 | 上海电力学院 | Organic reinforced concrete corrosion inhibitor and preparation method thereof |
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