CN111334806B - Rust remover and preparation method and application thereof - Google Patents
Rust remover and preparation method and application thereof Download PDFInfo
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- CN111334806B CN111334806B CN202010202717.XA CN202010202717A CN111334806B CN 111334806 B CN111334806 B CN 111334806B CN 202010202717 A CN202010202717 A CN 202010202717A CN 111334806 B CN111334806 B CN 111334806B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/08—Iron or steel
- C23G1/083—Iron or steel solutions containing H3PO4
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Abstract
The invention provides a rust remover and a preparation method and application thereof. The rust remover comprises the following components in percentage by mass: 15-30% of phosphoric acid, 1-10% of hypophosphorous acid, 0.1-5% of sodium salt, 0.1-5% of composite surfactant and the balance of water; the composite surfactant comprises: alkylphenol ethoxylates, isomeric alcohol ethoxylates and nitric acid. The rust remover can efficiently and quickly remove rust, has high rust removing efficiency and short rust removing time, is simple in use method, slightly corrodes a base material, and has high glossiness of the surface of a workpiece after rust removal.
Description
Technical Field
The invention belongs to the technical field of steel rust removal, and particularly relates to a rust remover and a preparation method and application thereof.
Background
At present, the rust removal of steel products is mainly hydrochloric acid pickling. The traditional chemical rust removal usually uses strong acid, the acid can react with iron rust and metal oxide to generate soluble salt, so as to achieve the purpose of rust removal, and the acid can react with base metal to release hydrogen while removing rust, and the hydrogen can generate pressure on the iron rust and indissolvable oxide skin, thereby being beneficial to the peeling of the iron rust and the reduction of high-valence iron and accelerating the pickling process. But the traditional acid liquor treatment method also has obvious defects, and acid gas with strong irritation and corrosivity can be generated in the acid washing process; the acid liquid loses efficacy due to the rapid increase of iron ions, and waste acid is generated; in addition, the pickled workpieces are washed with water to remove residual acid solution, thus producing spent pickling water. The waste gas, waste liquid and waste acid washing water cause serious pollution of the prior acid washing rust removal, which is increasingly limited under the current environment-friendly high pressure. The existing environment-friendly phosphoric acid type rust remover has low rust removing efficiency, long-time ultrasound or heating to a high temperature of 50 ℃ is needed to accelerate the rust removing efficiency, the energy consumption is high, and certain corrosion can be generated on the metal surface by prolonging the treatment time.
CN105018947A discloses a rust remover, which is composed of 17-25% of citric acid, 0.5-10% of oxalic acid, 15-45% of phosphoric acid, 0.5-2% of sodium alkyl benzene sulfonate, 0.5-4% of emulsifier, 3.5-5.5% of corrosion inhibitor and the balance of deionized water, and has good rust removing effect on light rust, but has longer treatment time on oxide skin of a heavy rust belt, and is easy to damage the surface of the heavy rust belt.
CN109468647A discloses a rust remover, which comprises the following raw materials: the water-soluble calcium phosphate-containing composite material comprises, by mass, 15-30 parts of phosphoric acid, 20-50 parts of lauryl sodium sulfate, 15-40 parts of calcium hypophosphite, 5-50 parts of potassium tetraborate and 4-25 parts of ammonium molybdate. The invention can not cause corrosion or other damages to steel, can eliminate rust on the steel, and can accelerate the rust removal efficiency by adding long-time ultrasonic or heating to 50 ℃ high temperature, thereby not only having high energy consumption, but also generating certain corrosion to the metal surface by prolonging the treatment time.
Therefore, the research and development of the rust remover which is safer and more environment-friendly and has high rust removing efficiency is particularly important.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a rust remover, a preparation method and application thereof, wherein the rust remover belongs to a phosphoric acid series weak acid rust remover, generates little volatile gas in the using process, can efficiently and quickly remove rust, has high rust removing efficiency and short rust removing time, is simple in using method, has light corrosion on a base material, and has high glossiness of the surface of a workpiece after rust removal.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a rust remover, which comprises the following components in percentage by mass: 15-30% of phosphoric acid, 1-10% of hypophosphorous acid, 0.1-5% of sodium salt, 0.1-5% of composite surfactant and the balance of water;
the composite surfactant comprises: alkylphenol ethoxylates, isomeric alcohol ethoxylates and nitric acid.
In the present invention, the phosphoric acid content is 15 to 30%, and may be, for example, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%.
In the present invention, the hypophosphorous acid content is 1 to 10%, and may be, for example, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%.
In the present invention, the content of the sodium salt is 0.1 to 5%, and may be, for example, 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%.
In the present invention, the content of the composite surfactant is 0.1 to 5%, and may be, for example, 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%.
The rust remover disclosed by the invention belongs to a phosphoric acid weak acid rust remover, and volatile gas is rarely generated in the using process; because the rust removal is not carried out by the hydrochloric acid stripping type rust removal, but is carried out by the conversion type rust removal, the rust is converted into iron salt to be present on the surface of the workpiece. Thus, iron ions entering the rust removing liquid are greatly reduced, so that the service life of the rust removing agent is greatly prolonged, and the generation amount of waste liquid is greatly reduced; in addition, the rust remover does not need to wash iron ions attached to the surface of a workpiece, the amount of washing required is small, and the rust remover can be completely used for regenerating the rust remover or preparing a new rust remover; finally, the rust remover can be completely regenerated without generating secondary pollutants. Therefore, the environment-friendly rust remover rarely generates waste liquid and waste gas, and does not discharge waste acid washing water. Compared with hydrochloric acid rust removal, the environmental protection is greatly improved.
The components of the rust remover comprise phosphoric acid, hypophosphorous acid, sodium salt and a composite surfactant, and the components are matched with each other to realize synergistic interaction, so that the rust removing efficiency and the rust removing speed are effectively improved. The rust remover mainly comprises phosphoric acid which is weak in acidity, and is added with a composite surfactant to be matched with phosphoric acid, hypophosphorous acid and sodium salt components to improve the reaction rate. At the same time, the synergistic effect between the components of the composite surfactant enables free H+The corrosion (electrochemical corrosion and chemical corrosion) process of the exposed base metal surface after rust removal is slowed down, so that over-pickling and hydrogen embrittlement are avoided. Fe is generated in the solution after phosphoric acid rust removal3+And Fe2+In which Fe3+Iron phosphate precipitation with phosphate ions occurred, but the precipitation rate was low. Therefore, hypophosphorous acid and a composite surfactant are added, so that the deposition rate of the iron phosphate is improved.
Preferably, the sodium salt is a mixture of sodium fluoride and sodium nitrate. To better remove Fe in the solution3 +Sodium fluoride is added into the solution, and the sodium fluoride can be mixed with Fe3+Forming a soluble, colorless sodium hexafluoroiron (III) complex which further eliminates Fe3+Of Fe2O3+6H+＝2Fe3++3H2The O reaction moves in the forward direction. The sodium nitrate is used as a builder to promote the integration of the composite surfactant with metal ions and also promote the improvement of the cleaning capability of the composite surfactant on the metal surface rust.
Preferably, the mass ratio of the sodium fluoride to the sodium nitrate is (2-3) to (5-10). Within the proportion range, the sodium fluoride and the sodium nitrate are matched with each other, so that the synergistic effect is achieved, the effect of integrating metal ions by the composite surfactant can be further promoted, and the cleaning capability of the composite surfactant on metal surface rust can be further promoted.
Wherein, the 2-3 can be 2, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3.
Wherein, the 5-10 can be 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5 and 10.
Preferably, the mass ratio of the alkylphenol polyoxyethylene ether to the isomeric alcohol polyoxyethylene ether to the nitric acid is (4-5) to (1-2) to (2-3).
Wherein, the 4-5 can be 4, 4.1, 4.2, 4.3, 4.4, 4.5, 4.6, 4.7, 4.8, 4.9, 5.
Wherein, the 1-2 can be 1, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9 and 2.
Wherein, the 2-3 can be 2, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3.
Preferably, the alkylphenol ethoxylate is OP-10.
Preferably, the isomeric alcohol polyoxyethylene ether is isomeric decyl alcohol polyoxyethylene ether.
Preferably, the rust remover comprises the following components in percentage by mass: 15-30% of phosphoric acid, 1-10% of hypophosphorous acid, 0.4-0.6% of sodium fluoride, 1-2% of sodium nitrate, 100.8-1.0% of OP-100, 0.2-0.4% of isomeric dodecyl alcohol polyoxyethylene ether, 0.4-0.6% of nitric acid and the balance of water.
In the present invention, the sodium fluoride content may be 0.4 to 0.6%, for example, 0.4%, 0.42%, 0.44%, 0.46%, 0.48%, 0.5%, 0.52%, 0.54%, 0.56%, 0.58%, 0.6%.
In the present invention, the sodium nitrate content is 1 to 2%, and may be, for example, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, or 2%.
In the present invention, the content of OP-10 is 0.8 to 1.0%, and may be, for example, 0.8%, 0.82%, 0.84%, 0.86%, 0.88%, 0.9%, 0.92%, 0.94%, 0.96%, 0.98%, 1.0%.
In the present invention, the content of the isomeric polyoxyethylene lauryl ether is 0.2 to 0.4%, and may be, for example, 0.2%, 0.22%, 0.24%, 0.26%, 0.28%, 0.3%, 0.32%, 0.34%, 0.36%, 0.38%, or 0.4%.
In the present invention, the content of the nitric acid is 0.4 to 0.6%, and may be, for example, 0.4%, 0.42%, 0.44%, 0.46%, 0.48%, 0.5%, 0.52%, 0.54%, 0.56%, 0.58%, 0.6%.
Preferably, the rust remover comprises the following components in percentage by mass: 20-25% of phosphoric acid, 3-5% of hypophosphorous acid, 0.4-0.6% of sodium fluoride, 1-2% of sodium nitrate, 100.8-1.0% of OP-100, 0.2-0.4% of isomeric dodecyl alcohol polyoxyethylene ether, 0.4-0.6% of nitric acid and the balance of water.
In a second aspect, the present invention provides a method for preparing the rust remover as described in the first aspect, the method comprising: mixing and stirring phosphoric acid, hypophosphorous acid, sodium salt, a composite surfactant and water according to the formula amount to prepare the rust remover.
Preferably, the mixing and stirring temperature is 10-30 ℃, for example, 10 ℃, 12 ℃, 14 ℃, 16 ℃, 18 ℃, 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃, 30 ℃.
Preferably, the mixing and stirring speed is 300-600r/min, such as 300r/min, 320r/min, 340r/min, 360r/min, 380r/min, 400r/min, 420r/min, 440r/min, 460r/min, 480r/min, 500r/min, 520r/min, 540r/min, 560r/min, 580r/min, 600 r/min.
Preferably, the mixing and stirring time is 10-30min, such as 10min, 12min, 14min, 16min, 18min, 20min, 22min, 24min, 26min, 28min, 30 min.
Preferably, the preparation method comprises the following steps: according to the formula, phosphoric acid, hypophosphorous acid, sodium fluoride, sodium nitrate, OP-10, isomeric dodecyl polyoxyethylene ether, nitric acid and water are mixed and stirred for 10-30min at the temperature of 10-30 ℃ and the rotating speed of 300-600r/min to prepare the rust remover.
In a third aspect, the invention provides a use of the rust remover as described in the first aspect for removing rust from the surface of a steel product.
The rust remover provided by the invention can remove rust at normal temperature under ultrasonic waves, and the ultrasonic power can be 400-800W, such as 400W, 450W, 500W, 550W, 600W, 650W, 700W, 750W, 800W and the like.
The rust remover provided by the invention can remove rust under heating without ultrasonic treatment, and the heating temperature can be 40-60 ℃, for example, 40 ℃, 42 ℃, 44 ℃, 46 ℃, 48 ℃, 50 ℃, 52 ℃, 54 ℃, 56 ℃, 58 ℃, 60 ℃ and the like.
Compared with the prior art, the invention has the following beneficial effects:
(1) the rust remover can remove rust on metal, can effectively protect metal base materials, reduce corrosion of the metal base materials, reduce harm of hydrogen embrittlement to workpieces, has a rust removing rate of over 99 percent, high rust removing speed and high rust removing efficiency, is simple in use method, slightly corrodes the base materials, and has high surface glossiness of the workpieces after rust removal.
(2) The rust remover provided by the invention utilizes conversion rust removal instead of stripping rust removal, so that the service life of the rust remover is prolonged, the discharge amount of the rust remover is greatly reduced, zero discharge can be realized through regeneration treatment, and the rust remover has the advantages of low water consumption, capability of realizing preparation or regeneration balance with fresh acid, no wastewater discharge and environmental friendliness.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
OP-10 (polyoxyethylene octylphenol ether, manufactured by Tengjin, Yin commercial Co., Ltd.) is used in the following examples; isomeric dodecyl alcohol polyoxyethylene ether (JFC, manufactured by Beijing Huasheng Ruiko chemical Co., Ltd.).
Example 1
The embodiment provides a rust remover, which comprises the following components in percentage by mass: 20% of phosphoric acid, 5% of hypophosphorous acid, 0.4% of sodium fluoride, 1% of sodium nitrate, OP-100.8%, 0.4% of isomeric dodecyl alcohol polyoxyethylene ether, 0.6% of nitric acid and the balance of deionized water.
The preparation method of the rust remover comprises the following steps: according to the formula, phosphoric acid, hypophosphorous acid, sodium fluoride, sodium nitrate, OP-10, isomeric dodecyl polyoxyethylene ether, nitric acid and water are mixed and stirred for 20min at the rotating speed of 400r/min at the temperature of 20 ℃ to prepare the rust remover.
Example 2
The embodiment provides a rust remover, which comprises the following components in percentage by mass: 25% of phosphoric acid, 3% of hypophosphorous acid, 0.6% of sodium fluoride, 2% of sodium nitrate, OP-101.0%, 0.2% of isomeric dodecyl alcohol polyoxyethylene ether, 0.4% of nitric acid and the balance of deionized water.
The preparation method of the rust remover comprises the following steps: according to the formula, phosphoric acid, hypophosphorous acid, sodium fluoride, sodium nitrate, OP-10, isomeric dodecyl polyoxyethylene ether, nitric acid and water are mixed and stirred at the rotating speed of 600r/min for 10min at the temperature of 10 ℃ to prepare the rust remover.
Example 3
The embodiment provides a rust remover, which comprises the following components in percentage by mass: 22% of phosphoric acid, 4% of hypophosphorous acid, 0.5% of sodium fluoride, 1.5% of sodium nitrate, 100.9% of OP-100, 0.3% of isomeric dodecyl alcohol polyoxyethylene ether, 0.5% of nitric acid and the balance of deionized water.
The preparation method of the rust remover comprises the following steps: mixing and stirring phosphoric acid, hypophosphorous acid, sodium fluoride, sodium nitrate, OP-10, isomeric dodecyl polyoxyethylene ether, nitric acid and water at the temperature of 30 ℃ at the rotating speed of 300r/min for 30min according to the formula ratio to prepare the rust remover.
Example 4
This example provides a rust remover, which is different from example 1 in that the content of sodium fluoride is 1%, the content of sodium nitrate is 0.4%, and the content of other components and the preparation method are not changed.
Example 5
This example provides a rust remover, which is different from example 1 in that the content of sodium fluoride is 0.2%, the content of sodium nitrate is 1.2%, and the content of other components and the preparation method are not changed.
Example 6
This example provides a rust remover, which is different from example 1 in that the rust remover does not contain sodium fluoride, the content of sodium nitrate is increased to 1.4%, and the contents of other components and the preparation method are not changed.
Example 7
This example provides a rust remover, which is different from example 1 in that the rust remover does not contain sodium nitrate, the content of sodium fluoride is increased to 1.4%, and the content of other components and the preparation method are not changed.
Example 8
This example provides a rust remover, which is different from example 1 in that OP-100.6%, isomeric dodecyl alcohol polyoxyethylene ether 0.6% and nitric acid 0.6%, and the contents of other components and preparation method are unchanged.
Comparative example 1
This comparative example provides a rust remover, which is different from example 1 in that hypophosphorous acid was not added, the phosphoric acid content was increased to 25%, and the contents of other components and the preparation method were not changed.
Comparative example 2
This comparative example provides a rust remover which is different from example 1 in that no sodium salt is added, the phosphoric acid content is increased to 21.4%, and the contents of other components and the preparation method are not changed.
Comparative example 3
This comparative example provides a rust remover, which is different from example 1 in that the rust remover does not add a composite surfactant, the phosphoric acid content is increased to 21.8%, and the contents of other components and the preparation method are not changed.
Comparative example 4
The comparative example provides a rust remover, which is different from the rust remover in example 1 in that no OP-10 is added, the content of isomeric dodecyl alcohol polyoxyethylene ether is increased to 0.8%, the content of nitric acid is increased to 1.0%, and the content of other components and the preparation method are not changed.
Comparative example 5
This comparative example provides a rust remover, which is different from example 1 in that isomeric deca-alcohol polyoxyethylene ether was not added to the rust remover, the OP-10 content was increased to 1.0%, the nitric acid content was increased to 0.8%, and the contents of other components and the preparation method were not changed.
Comparative example 6
This comparative example provides a rust remover, which is different from example 1 in that nitric acid is not added to the rust remover, the OP-10 content is increased to 1.1%, the isomeric dodecyl alcohol polyoxyethylene ether content is increased to 0.7%, and the contents of other components and the preparation method are not changed.
Comparative example 7
This comparative example provides a rust remover, which is different from example 1 in that OP-10 was replaced with AEO-9, and the contents of other components and the preparation method were not changed.
Comparative example 8
The comparative example provides a rust remover, which is different from the rust remover in example 1 in that isomeric dodecyl polyoxyethylene ether is replaced by sodium dodecyl benzene sulfonate, and the content of other components and the preparation method are not changed.
Comparative example 9
This comparative example provides a rust remover, which is different from example 1 in that nitric acid is replaced with sulfuric acid, and the contents of other components and the preparation method are not changed.
Test examples
The rust removers prepared in the above examples 1 to 8 and the rust removers prepared in the comparative examples 1 to 9 were subjected to performance test experiments, and the test process was as follows: respectively adding a rust remover into a water tank of an ultrasonic machine, immersing the steel piece to be cleaned into the rust remover, starting ultrasonic treatment, and carrying out rust removal treatment under the conditions that the ultrasonic rated power is 800W at the temperature of 20 ℃; or the water tank is heated to 50 ℃ and directly derusted without ultrasonic treatment, and the rust removal rate and the rust removal time are shown in table 1.
TABLE 1
From the test data, the rust removal rate of the rust remover prepared in the examples 1-8 is more than 95%, the ultrasonic rust removal time is within 20min, the heating rust removal time at 30 ℃ is within 35min, and the glossiness is more than 90%, so that the rust remover has the advantages of higher rust removal rate, shorter rust removal time and higher glossiness of the surface of a cleaned workpiece compared with the rust remover prepared in the comparative examples 1-9. The components of the rust remover are matched with each other, so that the rust remover can remove rust on metal, has an obvious rust removing effect, is simple in using method, slightly corrodes a base material, and is high in glossiness after rust removal.
In the examples 1-3, the rust removal rate can reach more than 99% as an optimal technical scheme, the rust removal time is short, and the rust removal efficiency is high. Whereas the rust remover prepared in example 4 with too little sodium nitrate or in example 6 without sodium nitrate slightly decreased the cleaning ability to rust on the metal surface due to lack of the effect of promoting the integration of metal ions by the composite surfactant, example 5 with too little sodium fluoride or example 7 without sodium fluoride, Fe after dissolution of rust by acid3+Cannot generate soluble sodium hexafluoroiron (III) complex and cannot eliminate Fe3+Therefore, the rust removal rate is slightly decreased.
The applicant states that the present invention is illustrated by the above examples to the rust remover of the present invention and the preparation method and application thereof, but the present invention is not limited to the above examples, that is, it does not mean that the present invention must be implemented by relying on the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (4)
1. The rust remover is characterized by comprising the following components in percentage by mass: 15-30% of phosphoric acid, 1-10% of hypophosphorous acid, 0.4-0.6% of sodium fluoride, 1-2% of sodium nitrate, 100.8-1.0% of OP-100, 0.2-0.4% of isomeric dodecyl alcohol polyoxyethylene ether, 0.4-0.6% of nitric acid and the balance of water.
2. The rust remover as claimed in claim 1, characterized in that the rust remover consists of the following components in percentage by mass: 20-25% of phosphoric acid, 3-5% of hypophosphorous acid, 0.4-0.6% of sodium fluoride, 1-2% of sodium nitrate, 100.8-1.0% of OP-100, 0.2-0.4% of isomeric dodecyl alcohol polyoxyethylene ether, 0.4-0.6% of nitric acid and the balance of water.
3. A method for producing a rust remover according to claim 1 or 2, characterized by comprising: according to the formula, phosphoric acid, hypophosphorous acid, sodium fluoride, sodium nitrate, OP-10, isomeric dodecyl polyoxyethylene ether, nitric acid and water are mixed and stirred for 10-30min at the temperature of 10-30 ℃ and the rotating speed of 300-600r/min to prepare the rust remover.
4. Use of the rust remover according to claim 1 or 2 for removing rust from the surface of a steel product.
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| CN115961287A (en) * | 2022-12-28 | 2023-04-14 | 广东红日星实业有限公司 | Film removing agent and preparation method and application thereof |
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