CN108395133B - Preparation method of long-acting corrosion-resistant reinforcing steel bar rust inhibitor material - Google Patents
Preparation method of long-acting corrosion-resistant reinforcing steel bar rust inhibitor material Download PDFInfo
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- CN108395133B CN108395133B CN201810306609.XA CN201810306609A CN108395133B CN 108395133 B CN108395133 B CN 108395133B CN 201810306609 A CN201810306609 A CN 201810306609A CN 108395133 B CN108395133 B CN 108395133B
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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
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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
- 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 relates to a preparation method of a long-acting corrosion-resistant reinforcing steel bar rust inhibitor material, belonging to the technical field of rust inhibitor materials. According to the technical scheme, the dunaliella salina is extracted, alcohol extracts of the dunaliella salina are collected and grafted with amino acid materials, meanwhile, chitosan and water are mixed to form gel and coat the grafted modified materials, the gel layer formed by the alcohol substances is loaded to the surface of a steel bar material to form a passivation film, the formed passivation film material has excellent passivation formation, corrosion of the steel bar material is effectively organized, and the corrosion resistance of the material is improved.
Description
Technical Field
The invention relates to a preparation method of a long-acting corrosion-resistant reinforcing steel bar rust inhibitor material, belonging to the technical field of rust inhibitor materials.
Background
Since Portland cement appeared in the 20 th of the 19 th century, concrete materials had been used for over 100 years since
The concrete has the advantages of large structural rigidity, easy construction, low construction cost, low later maintenance cost and the like, is the first choice material in the civil engineering structural design, and the consumption of the concrete in 1997 all over the world reaches 88 hundred million tons. In fact, during the more than 100 years since the concrete application in civil engineering, a large number of reinforced concrete structures have failed in advance for various reasons, failing to reach the predetermined service life. Some of these are due to insufficient resistance of the structural design, some are due to adverse changes in service loads, but more are due to failure due to insufficient durability of the structure. In particular, concrete structures in coastal and offshore areas are damaged early due to corrosion of steel bars caused by corrosion of concrete in marine environments, and the durability of the structures is lost, which is an important problem in practical engineering.
The steel bar corrosion inhibitor is mainly used for improving and enhancing the corrosion resistance of steel bars through chemical and electrochemical actions. The main function of the steel bar corrosion inhibitor is not to prevent chloride ions in the environment from entering the concrete, and the essence of the steel bar corrosion inhibitor is to inhibit, prevent and delay the electrochemical process of steel bar corrosion. Generally speaking, the higher the content of the rust inhibitor in the concrete, the higher the amount of chloride ions allowed to enter without rusting the reinforcing steel bars, so that the 'critical value' of the corrosion of the reinforcing steel bars by the chloride ions is increased, and the comprehensive result is that the time of salt damage is delayed and the development speed is delayed, thereby achieving the purpose of prolonging the service life of the structure. It mainly plays the rust inhibition effect through three aspects and protects the reinforcing bar: (1) forming a barrier layer; (2) surface passivation by oxidation; (3) affecting the environment of the medium in contact with the concrete reinforcing bars. However, the rust inhibitor of the existing rust inhibitor material has low durable rust resistance and affects the use prospect of the rust inhibitor material, so that how to prepare the long-lasting and stable reinforcing steel bar rust inhibitor is necessary.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems that the existing rust inhibitor material has insufficient rust inhibition performance and has influence on the use prospect of the rust inhibitor material, the preparation method of the long-acting corrosion-resistant reinforcing steel bar rust inhibitor material is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
(1) taking dunaliella salina, washing and drying, collecting dry dunaliella salina particles, adding the dry dunaliella salina particles into ethyl acetate according to the mass ratio of 1:10, soaking for 6-8 hours, filtering, collecting filter cakes, washing and drying to obtain degreased dunaliella salina particles;
(2) respectively weighing 45-50 parts by weight of deionized water, 10-15 parts by weight of degreased dunaliella salina particles, 3-5 parts by weight of zinc chloride and 10-15 parts by weight of disodium hydrogen phosphate solution, stirring and mixing, heating in a water bath for 3-5 hours, standing, cooling to room temperature, filtering, and collecting filtrate to obtain modified solution;
(3) adding chitosan into the modified solution according to the mass ratio of 1:5, stirring and mixing to obtain a mixed solution, respectively weighing 45-50 parts of the mixed solution, 3-5 parts of glycine and 1-2 parts of 0.5mol/L sodium hydroxide solution in parts by weight, placing the mixed solution, the glycine and the sodium hydroxide solution into a three-neck flask, stirring and mixing, introducing nitrogen to remove air, heating in a water bath, standing and cooling to room temperature, collecting the reaction solution, and performing rotary evaporation to obtain a concentrated solution;
(4) respectively weighing 45-50 parts by weight of deionized water, 10-15 parts by weight of concentrated solution, 3-5 parts by weight of zinc oxide, 3-5 parts by weight of titanium oxide, 6-8 parts by weight of fatty alcohol-polyoxyethylene ether sodium sulfate and 6-8 parts by weight of calcium hydroxy phosphate, placing the materials in a mortar, grinding and dispersing at room temperature, and collecting dispersed slurry to prepare the long-acting corrosion-resistant reinforcing steel bar rust inhibitor material.
And (3) the disodium hydrogen phosphate solution in the step (2) is a disodium hydrogen phosphate solution with the mass fraction of 10%.
And (4) introducing the nitrogen at a rate of 45-50 mL/min in the step (3).
And (3) carrying out rotary evaporation at 45-50 ℃ until the volume of the reaction solution is 1/5.
Compared with other methods, the method has the beneficial technical effects that:
(1) according to the technical scheme, the dunaliella salina is extracted, alcohol extracts of the dunaliella salina are collected and grafted with amino acid materials, meanwhile, chitosan and water are mixed to form gel and coat the grafted modified materials, the gel layer formed by the alcohol substances is loaded to the surface of a steel bar material to form a passivation film, the formed passivation film material has excellent passivation formation, corrosion of the steel bar material is effectively organized, and the corrosion resistance of the material is improved;
(2) the technical scheme of the invention is that the amino modified rust inhibitor prepared by the method has good reduction performance, partial ions are displaced from the surface of iron oxide in an anode region to be passivated on the surface of a steel bar to form a film, the rust inhibitor reaches the surface of the steel bar by diffusion, hydrophobic groups of polar groups such as N, S, OH & lt- & gt are combined with organic high molecular compounds such as hydrocarbon chains and the like, and simultaneously act on a cathode and an anode, iron atoms or iron ions are fixed by strong physical or chemical adsorption force of unshared electrons, the critical chloride ion concentration value is improved, the generated chelate ring replaces Cl & lt- & gt, OH & lt- & gt and other anions originally adsorbed on the surface of the steel bar, molecular films are formed in both the cathode region and the anode region, and the corrosion of the steel bar is inhibited.
Detailed Description
Taking dunaliella salina, washing the dunaliella salina with deionized water for 3-5 times, carrying out vacuum freeze drying, collecting dried dunaliella salina particles, adding the dried dunaliella salina particles into ethyl acetate according to a mass ratio of 1:10, soaking for 6-8 hours, filtering, collecting filter cakes, washing with deionized water for 3-5 times, drying at 55-60 ℃ for 6-8 hours to obtain defatted dunaliella salina particles, respectively weighing 45-50 parts by weight of deionized water, 10-15 parts by weight of defatted dunaliella salina particles, 3-5 parts by weight of zinc chloride and 10-15 parts by weight of 10% disodium hydrogen phosphate solution, stirring, mixing, heating in a water bath at 120-130 ℃ for 3-5 hours, standing, cooling to room temperature, filtering, and collecting filtrate to obtain a modified solution; adding chitosan into the modified solution according to the mass ratio of 1:5, stirring and mixing to obtain a mixed solution, respectively weighing 45-50 parts of the mixed solution, 3-5 parts of glycine and 1-2 parts of 0.5mol/L sodium hydroxide solution in parts by weight, placing the mixed solution, the glycine and the sodium hydroxide solution into a three-neck flask, stirring and mixing, introducing nitrogen to remove air, controlling the introduction rate of the nitrogen to be 45-50 mL/min, heating the mixed solution in a water bath at 75-80 ℃ for 6-8 h, standing and cooling to room temperature, collecting the reaction solution, placing the reaction solution into a mortar at 45-50 ℃ for rotary evaporation to 1/5 of the volume of the reaction solution to obtain a concentrated solution, respectively weighing 45-50 parts of deionized water, 10-15 parts of the concentrated solution, 3-5 parts of zinc oxide, 3-5 parts of titanium oxide, 6-8 parts of sodium alcohol ether sulfate and 6-8 parts of calcium hydroxy phosphate in parts by weight, placing the mortar into the mortar, grinding and dispersing at room temperature and collecting dispersed slurry, the long-acting corrosion-resistant reinforcing steel bar rust inhibitor material can be prepared.
Taking dunaliella salina, washing the dunaliella salina for 3 times by using deionized water, carrying out vacuum freeze drying and collecting dried dunaliella salina particles, adding the dried dunaliella salina particles into ethyl acetate according to the mass ratio of 1:10, soaking for 6 hours, filtering and collecting filter cakes, washing the filter cakes for 3 times by using the deionized water, then drying the filter cakes for 6 hours at 55 ℃ to obtain degreased dunaliella salina particles, respectively weighing 45 parts of the deionized water, 10 parts of the degreased dunaliella salina particles, 3 parts of zinc chloride and 10 parts of 10 mass percent disodium hydrogen phosphate solution according to parts by weight, stirring and mixing the materials, heating the mixture in a water bath at 120 ℃ for 3 hours, standing, cooling the mixture to room temperature, filtering the mixture, and collecting filtrate to obtain modified liquid; adding chitosan into the modified solution according to the mass ratio of 1:5, stirring and mixing to obtain a mixed solution, respectively weighing 45 parts of the mixed solution, 3 parts of glycine and 1 part of 0.5mol/L sodium hydroxide solution by weight, placing the mixed solution, the 3 parts of glycine and the 1 part of 0.5mol/L sodium hydroxide solution into a three-neck flask, stirring and mixing, introducing nitrogen to remove air, controlling the nitrogen introduction rate to be 45mL/min, heating the mixed solution in a water bath at 75 ℃ for 6 hours, standing and cooling the mixed solution to room temperature, collecting the reaction solution, placing the reaction solution into 1/5 of the volume of the reaction solution through rotary evaporation at 45 ℃ to obtain a concentrated solution, respectively weighing 45 parts of deionized water, 10 parts of the concentrated solution, 3 parts of zinc oxide, 3 parts of titanium oxide, 6 parts of sodium alcohol ether sulfate and 6 parts of calcium hydroxy phosphate by weight, placing the concentrated solution into a mortar, grinding and dispersing at room temperature and collecting the dispersed slurry to obtain the long-acting corrosion-resistant reinforcing steel bar rust inhibitor material.
Taking dunaliella salina, washing the dunaliella salina for 4 times by using deionized water, carrying out vacuum freeze drying and collecting dried dunaliella salina particles, adding the dried dunaliella salina particles into ethyl acetate according to the mass ratio of 1:10, soaking for 7 hours, filtering, collecting filter cakes, washing the filter cakes for 4 times by using the deionized water, drying the filter cakes at 57 ℃ for 7 hours to obtain degreased dunaliella salina particles, respectively weighing 47 parts by weight of the deionized water, 12 parts by weight of the degreased dunaliella salina particles, 4 parts by weight of zinc chloride and 12 parts by weight of 10% disodium hydrogen phosphate solution, stirring, mixing, heating the mixture in a water bath at 128 ℃ for 4 hours, standing, cooling to room temperature, filtering, and collecting filtrate to obtain modified liquid; adding chitosan into the modified solution according to the mass ratio of 1:5, stirring and mixing to obtain a mixed solution, respectively weighing 47 parts of the mixed solution, 4 parts of glycine and 2 parts of 0.5mol/L sodium hydroxide solution according to the parts by weight, placing the mixed solution, 4 parts of glycine and 2 parts of 0.5mol/L sodium hydroxide solution into a three-neck flask, stirring and mixing, introducing nitrogen to remove air, controlling the nitrogen introduction rate to be 47mL/min, heating the mixed solution in a water bath at 77 ℃ for 7 hours, standing and cooling the mixed solution to room temperature, collecting the reaction solution, placing the reaction solution into 1/5 of the volume of the reaction solution through rotary evaporation at 47 ℃ to obtain a concentrated solution, respectively weighing 47 parts of deionized water, 12 parts of the concentrated solution, 4 parts of zinc oxide, 4 parts of titanium oxide, 7 parts of sodium alcohol ether sulfate and 7 parts of calcium hydroxy phosphate according to the parts by weight, placing the mixed solution into a mortar, grinding and dispersing at room temperature and collecting the dispersed slurry to obtain the long-acting corrosion-resistant reinforcing steel bar rust inhibitor material.
Taking dunaliella salina, washing the dunaliella salina for 5 times by using deionized water, carrying out vacuum freeze drying and collecting dried dunaliella salina particles, adding the dried dunaliella salina particles into ethyl acetate according to the mass ratio of 1:10, soaking for 8 hours, filtering and collecting filter cakes, washing the filter cakes for 5 times by using the deionized water, drying the filter cakes at 60 ℃ for 8 hours to obtain degreased dunaliella salina particles, respectively weighing 50 parts by weight of the deionized water, 15 parts by weight of the degreased dunaliella salina particles, 5 parts by weight of zinc chloride and 15 parts by weight of 10% disodium hydrogen phosphate solution, stirring and mixing the materials, heating the mixture in a water bath at 130 ℃ for 5 hours, standing, cooling the mixture to room temperature, filtering the mixture, and collecting filtrate to obtain modified liquid; adding chitosan into the modified solution according to the mass ratio of 1:5, stirring and mixing to obtain a mixed solution, respectively weighing 50 parts of the mixed solution, 5 parts of glycine and 2 parts of 0.5mol/L sodium hydroxide solution according to the parts by weight, placing the mixed solution, 5 parts of glycine and 2 parts of 0.5mol/L sodium hydroxide solution into a three-neck flask, stirring and mixing, introducing nitrogen to remove air, controlling the nitrogen introduction rate to be 50mL/min, heating the mixed solution in a water bath at 80 ℃ for 8 hours, standing and cooling the mixed solution to room temperature, collecting the reaction solution, placing the reaction solution into 1/5 of the volume of the reaction solution through rotary evaporation at 50 ℃ to obtain a concentrated solution, respectively weighing 50 parts of deionized water, 15 parts of the concentrated solution, 5 parts of zinc oxide, 5 parts of titanium oxide, 8 parts of sodium alcohol ether sulfate and 8 parts of calcium hydroxy phosphate according to the parts by weight, placing the mixed solution into a mortar, grinding and dispersing at room temperature and collecting the dispersed slurry to obtain the long-acting corrosion-resistant reinforcing steel bar rust inhibitor material.
The performance of the prepared rust inhibitor material is tested, according to the technical specification of using the steel bar rust inhibitor (YB/T9231-2009), the steel bars of the steel bars prepared in the examples 1, 2 and 3 have a natural potential value of 120-135 mV after 7 days, the steel bars are not corroded, the steel bar rust inhibitor has excellent rust resistance, test pieces with the age of 15 months are taken, the surfaces of the test pieces are cleaned up, the test pieces are split by a concrete press, the steel bars are exposed in a bare mode, the test pieces with the steel bars not corroded are collected, the test pieces are placed into an aqueous solution containing 3% of sodium chloride to be soaked for 7 days, corrosion of the steel bars is not found, and the steel bar corrosion inhibitor has excellent corrosion resistance and long-acting performance after the reinforcement time reaches 28 days.
Claims (3)
1. A preparation method of a corrosion-resistant reinforcing steel bar rust inhibitor material is characterized by comprising the following specific preparation steps:
(1) taking dunaliella salina, washing and drying, collecting dry dunaliella salina particles, adding the dry dunaliella salina particles into ethyl acetate according to the mass ratio of 1:10, soaking for 6-8 hours, filtering, collecting filter cakes, washing and drying to obtain degreased dunaliella salina particles;
(2) respectively weighing 45-50 parts by weight of deionized water, 10-15 parts by weight of degreased dunaliella salina particles, 3-5 parts by weight of zinc chloride and 10-15 parts by weight of 10% disodium hydrogen phosphate solution, stirring and mixing, heating in a water bath for 3-5 hours, standing, cooling to room temperature, filtering, and collecting filtrate to obtain modified solution;
(3) adding chitosan into the modified solution according to the mass ratio of 1:5, stirring and mixing to obtain a mixed solution, respectively weighing 45-50 parts of the mixed solution, 3-5 parts of glycine and 1-2 parts of 0.5mol/L sodium hydroxide solution in parts by weight, placing the mixed solution, the glycine and the sodium hydroxide solution into a three-neck flask, stirring and mixing, introducing nitrogen to remove air, heating in a water bath, standing and cooling to room temperature, collecting the reaction solution, and performing rotary evaporation to obtain a concentrated solution;
(4) respectively weighing 45-50 parts by weight of deionized water, 10-15 parts by weight of concentrated solution, 3-5 parts by weight of zinc oxide, 3-5 parts by weight of titanium oxide, 6-8 parts by weight of fatty alcohol-polyoxyethylene ether sodium sulfate and 6-8 parts by weight of calcium hydroxy phosphate, placing the materials in a mortar, grinding and dispersing at room temperature, and collecting dispersed slurry to prepare the corrosion-resistant reinforcing steel bar rust inhibitor material.
2. The preparation method of the corrosion-resistant reinforcing steel bar rust inhibitor material according to claim 1, characterized by comprising the following steps: and (4) introducing the nitrogen at a rate of 45-50 mL/min in the step (3).
3. The preparation method of the corrosion-resistant reinforcing steel bar rust inhibitor material according to claim 1, characterized by comprising the following steps: and (3) carrying out rotary evaporation at 45-50 ℃ until the volume of the reaction solution is 1/5.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304178A (en) * | 2013-05-17 | 2013-09-18 | 河海大学 | Kelp extracting solution steel bar corrosion inhibitor and application thereof |
| CN105399783A (en) * | 2015-11-10 | 2016-03-16 | 江苏苏博特新材料股份有限公司 | Osamine organic rebar corrosion inhibitor and preparation method thereof |
| CN106082748A (en) * | 2016-06-26 | 2016-11-09 | 陈毅忠 | A kind of preparation method of biological reinforcing steel bar corrosion inhibitor |
| CN106366139A (en) * | 2016-08-29 | 2017-02-01 | 江苏苏博特新材料股份有限公司 | Aminoketose organic steel bar corrosion inhibitor and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304178A (en) * | 2013-05-17 | 2013-09-18 | 河海大学 | Kelp extracting solution steel bar corrosion inhibitor and application thereof |
| CN105399783A (en) * | 2015-11-10 | 2016-03-16 | 江苏苏博特新材料股份有限公司 | Osamine organic rebar corrosion inhibitor and preparation method thereof |
| CN106082748A (en) * | 2016-06-26 | 2016-11-09 | 陈毅忠 | A kind of preparation method of biological reinforcing steel bar corrosion inhibitor |
| CN106366139A (en) * | 2016-08-29 | 2017-02-01 | 江苏苏博特新材料股份有限公司 | Aminoketose organic steel bar corrosion inhibitor and preparation method thereof |
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Effective date of registration: 20211105 Address after: 101102, Tongzhou District Zhongguancun science and Technology Park, Tongzhou Park, Jinqiao Technology Industrial base, No. 12 middle section of Ring Road, Beijing Patentee after: BEIJING XINGTAI STEEL WELDMESH & TECHNOLOGY DEVELOPMENT Co.,Ltd. Address before: 213000 room 1102, unit 16, Hualin home, Bell Tower District, Changzhou, Jiangsu Patentee before: Wu Yaqin |
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