CN110819149A - Fibrous rare earth antirust pigment and preparation method thereof - Google Patents
Fibrous rare earth antirust pigment and preparation method thereof Download PDFInfo
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- CN110819149A CN110819149A CN201911278290.5A CN201911278290A CN110819149A CN 110819149 A CN110819149 A CN 110819149A CN 201911278290 A CN201911278290 A CN 201911278290A CN 110819149 A CN110819149 A CN 110819149A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/082—Anti-corrosive paints characterised by the anti-corrosive pigment
- C09D5/084—Inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/082—Anti-corrosive paints characterised by the anti-corrosive pigment
- C09D5/086—Organic or non-macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5317—Phosphonic compounds, e.g. R—P(:O)(OR')2
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Abstract
The invention discloses a fibrous rare earth antirust pigment and a preparation method thereof, wherein the method comprises the following steps: respectively dissolving amino trimethylene phosphonic acid and rare earth inorganic salt in water, wherein the concentration of the amino trimethylene phosphonic acid and the rare earth inorganic salt is 0.01-3 mol/L; adjusting the pH value of the amino trimethylene phosphonic acid solution to 4-7 by using alkali, and adding 0.01-0.5% of dispersing agent into the amino trimethylene phosphonic acid solution; proportioning according to the stoichiometric ratio of the reaction, and fully mixing amino trimethylene phosphonic acid and rare earth inorganic salt solution for reaction; standing the mixture, filtering, washing the precipitate with distilled water, and washing with deionized water to eliminate excessive inorganic salt ions; and drying the precipitate at 40-80 ℃ to obtain the fibrous rare earth antirust pigment. The invention has the advantages that: the coating can improve the corrosion resistance of the coating, and play a role of reinforcing short fibers to improve the wear resistance and strength of the coating.
Description
Technical Field
The invention belongs to the technical field of antirust pigments, and particularly relates to a fibrous rare earth antirust pigment and a preparation method thereof.
Background
Metallic materials have a wide range of applications, however, metal corrosion is a non-negligible problem in its application. Among the many corrosion protection measures, coating is one of the most common methods. The rust-preventive pigment is an important factor affecting the protective effect of the anticorrosive paint. Although conventional rust inhibitive pigments represented by red lead and zinc chrome yellow have a good rust inhibitive effect, toxic rust inhibitive pigments containing lead and chromium have been abandoned due to increasing human attention to the environment and health. Therefore, the development of a novel green and environmentally friendly rust preventive pigment is an important issue in this field. Rare earth salts represented by cerium and lanthanum are attracting attention because of their corrosion inhibiting effect, and their sparingly soluble Organic acid salt is expected to be a new generation of rust preventive pigment and has been studied intensively (Progress in Organic Coatings,2014, 77(4), 765-773.). For example, patent CN201310617421.4 (a chromium-free environment-friendly paint based on organic acid radical rare earth salt pigment and a preparation method) discloses a paint composition using organic acid radical rare earth salt pigment such as cerium cinnamate, cerium tartrate, cerium citrate, cerium malate, cerium salicylate, etc. However, the shape of the rust inhibitive pigment is generally spherical particles or flakes. Related researches find that the short fiber filler can reinforce the coating and improve the wear resistance and strength of the coating.
Therefore, the fibrous rare earth antirust pigment is developed, the antirust performance of the coating can be improved, the wear resistance and the strength of the coating are enhanced, and the fibrous rare earth antirust pigment has a high application prospect.
Disclosure of Invention
Aiming at the technical problems, the invention provides a fibrous rare earth antirust pigment and a preparation method thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a fibrous rare earth antirust pigment, in particular to a product of amino trimethylene phosphonic acid and rare earth inorganic salt. Wherein the chemical structure of the amino trimethylene phosphonic acid is as follows:
wherein the rare earth inorganic salt is one of cerium nitrate, lanthanum nitrate, cerium chloride and lanthanum chloride.
The preparation method of the fibrous rare earth antirust pigment comprises the following specific preparation processes:
(1) respectively dissolving amino trimethylene phosphonic acid and rare earth inorganic salt in water, wherein the concentration of the amino trimethylene phosphonic acid and the rare earth inorganic salt is 0.01-3 mol/L;
(2) adjusting the pH value of the amino trimethylene phosphonic acid solution to 4-7 by using alkali;
(3) adding 0.01-0.5% of dispersing agent into the amino trimethylene phosphonic acid solution;
(4) proportioning according to the stoichiometric ratio of the reaction, and fully mixing amino trimethylene phosphonic acid and rare earth inorganic salt solution for reaction;
(5) standing the mixture, filtering, washing the precipitate with distilled water, and washing with deionized water to eliminate excessive inorganic salt ions;
(6) and drying the precipitate at 40-80 ℃ to obtain the fibrous rare earth antirust pigment.
Wherein the alkali is common sodium hydroxide and potassium hydroxide.
Wherein the dispersant is polycarboxylic acid anionic dispersant.
The invention has the following advantages and beneficial effects: (1) the obtained antirust pigment has a large length-diameter ratio and has the characteristic of short fiber; (2) the obtained antirust pigment has double antirust effects of rare earth cations and amino trimethylene phosphonate anions.
In conclusion, the invention provides a novel fibrous rare earth antirust pigment which can improve the corrosion resistance of a coating, play a role of short fiber reinforcement and improve the wear resistance and strength of a coating.
Drawings
FIG. 1 is a morphology chart of a fibrous rare earth rust inhibitive pigment prepared by example 1 of the present invention;
FIG. 2 is a morphology chart of a fibrous rare earth rust inhibitive pigment prepared by example 2 of the present invention;
FIG. 3 is a morphology chart of a fibrous rare earth rust inhibitive pigment prepared by example 3 of the present invention;
FIG. 4 is a morphology chart of a fibrous rare earth rust inhibitive pigment prepared by example 4 of the present invention;
FIG. 5 is a morphological diagram of a rust inhibitive pigment prepared by comparative example 1 of the present invention;
FIG. 6 is a morphological diagram of a rust inhibitive pigment prepared by comparative example 2 of the present invention;
FIG. 7 is a graph showing the results of electrochemical polarization curve tests according to the present invention.
Detailed Description
The present invention is described in further detail below with reference to examples, which are intended to facilitate the understanding of the present invention and are not intended to limit the present invention in any way. The experimental methods in the following examples, which are not specified under specific conditions, are generally performed under conventional conditions. Unless otherwise indicated, all parts are parts by weight and all percentages are percentages by weight.
Example 1
0.01mol of aminotrimethylene phosphonic acid and 0.02mol of cerium nitrate were weighed out and dissolved in water, respectively. The pH of the aminotrimethylene phosphonic acid solution was adjusted to 6 with NaOH solution and then 0.01% Rohm and Haas 1124 dispersant was added to the aminotrimethylene phosphonic acid solution. Then, 0.01mol of aminotrimethylene phosphonic acid and 0.02mol of cerium nitrate solution were poured into a dispersion machine and stirred to be sufficiently mixed. The mixture is left to stand and filtered, and the precipitate is washed with distilled water and then washed with deionized water to eliminate possible excessive inorganic salt ions. Then the mixture is placed in an oven to be heated to 40 ℃ for drying, and the fibrous rare earth antirust pigment is obtained, and is shown in figure 1.
Example 2
0.01mol of aminotrimethylene phosphonic acid and 0.02mol of lanthanum nitrate were weighed out and dissolved in water, respectively. The pH of the aminotrimethylene phosphonic acid solution was adjusted to 6 with NaOH solution and then 0.01% Rohm and Haas 1124 dispersant was added to the aminotrimethylene phosphonic acid solution. Then, 0.01mol of aminotrimethylene phosphonic acid and 0.02mol of cerium nitrate solution were poured into a dispersion machine and stirred to be sufficiently mixed. The mixture is left to stand and filtered, and the precipitate is washed with distilled water and then washed with deionized water to eliminate possible excessive inorganic salt ions. Then the mixture is put in an oven to be heated to 40 ℃ for drying, and the fibrous rare earth antirust pigment is obtained, as shown in figure 2.
Example 3
3mol of aminotrimethylene phosphonic acid and 6mol of cerium nitrate were weighed out and dissolved in water, respectively. The pH of the aminotrimethylene phosphonic acid solution was adjusted to 6 with KOH solution and then 0.5% Rohm and Haas 1124 dispersant was added to the aminotrimethylene phosphonic acid solution. Then, 3mol of aminotrimethylene phosphonic acid and 6mol of cerium nitrate solution were poured into a dispersion machine and stirred to be sufficiently mixed. The mixture is left to stand and filtered, and the precipitate is washed with distilled water and then washed with deionized water to eliminate possible excessive inorganic salt ions. Then the mixture is put in an oven to be heated to 80 ℃ for drying, and the fibrous rare earth antirust pigment is obtained, as shown in figure 3.
Example 4
3mol of aminotrimethylene phosphonic acid and 6mol of lanthanum nitrate were weighed out and dissolved in water, respectively. The pH of the aminotrimethylene phosphonic acid solution was adjusted to 6 with KOH solution and then 0.5% Rohm and Haas 1124 dispersant was added to the aminotrimethylene phosphonic acid solution. Then 3mol of aminotrimethylene phosphonic acid and 6mol of lanthanum nitrate solution were poured into a dispersion machine and stirred to be mixed well. The mixture is left to stand and filtered, and the precipitate is washed with distilled water and then washed with deionized water to eliminate possible excessive inorganic salt ions. Then the mixture is put in an oven to be heated to 80 ℃ for drying, and the fibrous rare earth antirust pigment is obtained, as shown in figure 4.
Comparative example 1
0.01mol of aminotrimethylene phosphonic acid and 0.02mol of zinc nitrate were weighed out and dissolved in water, respectively. The pH of the aminotrimethylene phosphonic acid solution was adjusted to 6 with NaOH solution and then 0.01% Rohm and Haas 1124 dispersant was added to the aminotrimethylene phosphonic acid solution. Then, 0.01mol of aminotrimethylene phosphonic acid and 0.02mol of zinc nitrate solution were poured into a dispersion machine and stirred to be sufficiently mixed. The mixture is left to stand and filtered, and the precipitate is washed with distilled water and then washed with deionized water to eliminate possible excessive inorganic salt ions. Then the mixture is put in an oven and heated to 40 ℃ for drying, and the granular rare earth antirust pigment is obtained, as shown in figure 5.
Comparative example 2
0.01mol of phytic acid and 0.02mol of cerium nitrate were weighed and added to water, respectively, to dissolve them. The pH of the phytic acid solution was adjusted to 6 with KOH solution, then 0.5% rohm and haas 1124 dispersant was added to the phytic acid solution. Then 0.01mol of phytic acid and 0.02mol of cerium nitrate solution are poured into a dispersion machine to be stirred and fully mixed. The mixture is left to stand and filtered, and the precipitate is washed with distilled water and then washed with deionized water to eliminate possible excessive inorganic salt ions. Then the mixture is put in an oven and heated to 80 ℃ for drying, and the granular rare earth antirust pigment is obtained, as shown in figure 6.
And (3) corrosion inhibition effect characterization of the antirust pigment: the rust inhibitive pigment prepared in example 1 was immersed in a 3.5% NaCl solution for 24 hours to obtain an extract. Then, the leachate is used as electrolyte to carry out electrochemical polarization curve test. The measurement results are shown in fig. 7, and the comparison shows that the self-corrosion potential is shifted to the positive direction after the addition of the amino trimethylene cerium phosphonate, the corrosion tendency is reduced, and the self-corrosion current is also reduced, which indicates that the amino trimethylene cerium phosphonate prepared in example 1 has a good corrosion inhibition effect on carbon steel.
Characterization of the reinforcing effect of the fibrous rust-preventive pigment on the organic coating: 5 percent of rare earth antirust pigment is added into the water-based epoxy resin varnish and is uniformly dispersed. The coating was then brushed evenly onto a carbon steel plate with a brush and dried at room temperature, and the results were as follows.
1*The hardness of the paint film is determined according to GB T6739-2006 Pencil method for measuring color paint and varnish
2*According to GB/T9286-1998 test of marking out paint films of paints and varnishes
3*Method for measuring abrasion resistance of colored paint and varnish by GB/T1768-2006》
4*According to GB/T528-containing 2009 determination of tensile stress strain performance of vulcanized rubber or thermoplastic rubber
As can be seen from the table, compared with the granular antirust pigments of the zinc aminotrimethylene phosphonate and the cerium phytate, the wear resistance, the tensile strength and the elongation at break of the antirust pigments are obviously improved, and the fibrous rare earth antirust pigment is proved to be capable of obviously improving the comprehensive mechanical property of the coating.
The embodiments described above are intended to illustrate the technical solutions of the present invention, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modifications, additions, or equivalents made within the scope of the principles of the present invention should be included in the scope of the present invention.
Claims (5)
1. A fibrous rare earth antirust pigment is characterized by comprising the following specific components in percentage by weight: aminotrimethylene phosphonic acid and rare earth inorganic salts.
2. The fibrous rare earth rust inhibitive pigment according to claim 1, characterized in that: the chemical structure of the amino trimethylene phosphonic acid is as follows:
the rare earth inorganic salt is one of cerium nitrate, lanthanum nitrate, cerium chloride and lanthanum chloride.
3. A method for producing a fibrous rare earth rust inhibitive pigment according to claim 1, characterized by comprising the steps of:
(1) respectively dissolving amino trimethylene phosphonic acid and rare earth inorganic salt in water, wherein the concentration of the amino trimethylene phosphonic acid and the rare earth inorganic salt is 0.01-3 mol/L;
(2) adjusting the pH value of the amino trimethylene phosphonic acid solution to 4-7 by using alkali;
(3) adding 0.01-0.5% of dispersing agent into the amino trimethylene phosphonic acid solution;
(4) proportioning according to the stoichiometric ratio of the reaction, and fully mixing amino trimethylene phosphonic acid and rare earth inorganic salt solution for reaction;
(5) standing the mixture, filtering, washing the precipitate with distilled water, and washing with deionized water to eliminate excessive inorganic salt ions;
(6) and drying the precipitate at 40-80 ℃ to obtain the fibrous rare earth antirust pigment.
4. The process for producing a fibrous rare earth rust inhibitive pigment according to claim 3, wherein the alkali is common sodium hydroxide or potassium hydroxide.
5. The method for producing a fibrous rare earth anticorrosive pigment according to claim 3, wherein the dispersant is a polycarboxylic acid type anionic dispersant.
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| CN201911278290.5A CN110819149B (en) | 2019-12-13 | 2019-12-13 | Preparation method of fibrous rare earth antirust pigment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647300A (en) * | 2020-07-03 | 2020-09-11 | 南昌航空大学 | Anti-rust pigment for cathode electrophoretic coating and preparation method of slurry of anti-rust pigment |
| CN114539898A (en) * | 2022-03-03 | 2022-05-27 | 西安福莱特热处理有限公司 | Anticorrosive coating containing rare earth corrosion inhibitor HEDP-Ce and preparation method thereof |
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| CN103627298A (en) * | 2013-11-28 | 2014-03-12 | 中国科学院金属研究所 | Chromium-free environment-friendly paint based on organic acid radical rare-earth salt pigment and preparation method thereof |
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2019
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| US20130136944A1 (en) * | 2010-02-15 | 2013-05-30 | Productive Research Llc | Delamination resistant, weldable and formable light weight composites |
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| CN107592876A (en) * | 2015-04-08 | 2018-01-16 | 锌颜色的新公司 | The corrosion-inhibiting pigment made of polyphosphoric acid aluminium and rare earth |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647300A (en) * | 2020-07-03 | 2020-09-11 | 南昌航空大学 | Anti-rust pigment for cathode electrophoretic coating and preparation method of slurry of anti-rust pigment |
| CN114539898A (en) * | 2022-03-03 | 2022-05-27 | 西安福莱特热处理有限公司 | Anticorrosive coating containing rare earth corrosion inhibitor HEDP-Ce and preparation method thereof |
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| CN110819149B (en) | 2021-09-24 |
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