CN110451904B - Silane modified high-temperature-resistant anti-oxidation coating material and preparation method thereof - Google Patents
Silane modified high-temperature-resistant anti-oxidation coating material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of high-temperature-resistant coatings, and particularly relates to a silane-modified high-temperature-resistant anti-oxidation coating material and a preparation method thereof. The paint consists of the following components in parts by mass: nano SiO230.0 to 50.0 portions of nano Al2O36.0-8.0 parts of nano MgO 4.0-7.0 parts of nano TiO22.0-5.0 parts of silicon carbide SiC 15.0-25.0 parts of boron oxide B2O34.0 to 6.0 portions. According to the silane modified high-temperature-resistant anti-oxidation coating material, the metal oxide is used as the base material, and the aminosilane is used for treating the oxide powder, so that the oxide powder is more easily and uniformly dispersed in the coating and can stably exist, a foundation is laid for forming a uniform, compact and firmly-adhered coating, and the coating with an excellent protection effect is beneficial to improving the quality of hot-rolled steel.
Description
Technical Field
The invention belongs to the technical field of high-temperature-resistant coatings, and particularly relates to a silane-modified high-temperature-resistant anti-oxidation coating material and a preparation method thereof.
Background
With the continuous progress of social civilization, the demand of liquefied natural gas is rapidly increasing as a clean energy source. Nickel content of 9wt% steel material (9Ni steel) is widely used as a tank material for liquefied natural gas because of its advantages such as high strength and excellent fracture toughness in an ultra-low temperature environment. However, during the heat treatment process of the steel ingot with the section material (about 1250 ℃ for 60min), a thicker oxide layer is inevitably generated on the surface of the steel ingot, and the oxide layer is rich in nickel elements, so that the steel ingot is difficult to completely remove. If the phosphorus chips which are firmly adhered are not completely removed, the surface of the hot-rolled steel strip has defects of pits, stripes and the like, so that the product quality is influenced. In order to increase the yield of steel, the industry often adopts methods of heat treatment in a closed furnace, heat treatment in vacuum or gas protection, heat treatment in salt bath, polishing to remove a decarburized layer, increasing the heat treatment rate to prevent decarburization, protection of an antioxidant coating and the like, wherein the method of heat treatment by coating protection is simple in operation and low in cost, so that the attention is paid.
The research work of China on the aspect of the high-temperature protective coating of steel starts late, and the use effect of the high-temperature protective coating needs to be improved urgently, wherein the research work is caused by the laboratory environment and the industrial environment under the high-temperature conditionThe environment has a large difference, the research and development difficulty is large, and on the other hand, the problem that the suspension property and the stability of the coating are poor is difficult to solve. According to the literature and patents, the high temperature oxidation resistant coating material mainly comprises oxides (such as SiO) with different melting points2， Al2O3，MgO，TiO2And CaO, etc.) and functional components (e.g., SiC, B)2O3，ZrO2Graphite or carbon powder, etc.) and a binder (such as potassium silicate, sodium silicate, phosphate, etc.) in an amount exceeding 60 deg.fwtPercent; the high-temperature oxidation coating is obtained by uniformly mixing the coating materials and adding a proper amount of water or other organic solvents. Compared with the common coating, the components and the preparation method have the advantages that the stability of the high-temperature oxidation-resistant coating is poor, mainly because the components of the powder in the high-temperature oxidation-resistant coating are high, the content of the solvent is low, and meanwhile, the powder is difficult to be compatible with the binder or the solvent, so that the powder is difficult to be uniformly dispersed in the coating. If the powder in the coating is not uniformly dispersed, a storage-stable coating cannot be obtained, and a uniform and dense coating cannot be prepared.
Disclosure of Invention
Based on the heat treatment characteristics of the 9Ni steel, the invention combines the advantages of the existing high-temperature resistant protective coating and the obvious effect of silane on improving the powder dispersibility, solves the problem of uneven dispersion of the high-temperature resistant anti-oxidation coating material used in the hot rolling process of the existing 9Ni steel, provides a coating material which can be easily and uniformly dispersed and stably stored in a coating, and lays a foundation for obtaining a uniform and compact protective coating.
The invention is realized by the following technical scheme: a silane modified high-temperature-resistant oxidation-resistant coating material is composed of the following components in parts by mass:
nano SiO230.0 to 50.0 portions of nano Al2O36.0-8.0 parts of nano MgO 4.0-7.0 parts of nano TiO22.0-5.0 parts of silicon carbide SiC 15.0-25.0 parts of boron oxide B2O34.0 to 6.0 portions.
The invention further provides a preparation method of the silane modified high-temperature-resistant anti-oxidation coating material, which comprises the following steps:
a) preparing silane hydrolysis solution
(1) Weighing aminosilane, absolute ethyl alcohol and deionized water;
(2) under the condition of continuous stirring, firstly, adding absolute ethyl alcohol into aminosilane, and then slowly dropwise adding deionized water into a mixed solution of silane and ethyl alcohol;
(3) adjusting the pH value of the mixed solution to 9.0-10.0 by using ammonia water;
(4) placing the mixed solution in a water bath at 40 ℃, and continuously stirring to obtain a silane hydrolysis solution;
b) preparation of powder Material
(5) Weighing raw material powder according to the mass parts of the components of the silane-modified high-temperature-resistant anti-oxidation coating material, and uniformly stirring to obtain mixed powder;
(6) adding a silane hydrolysis solution into the mixed powder, and then carrying out ball milling to obtain mixed powder slurry;
(7) drying the powder slurry, and then cooling to room temperature to obtain dried mixed powder;
(8) and crushing the dried mixed powder, and then sieving for three times to obtain silane modified high-temperature-resistant anti-oxidation coating material powder.
Silane is a common external crosslinking reaction type crosslinking agent, and because the structure simultaneously contains an organic functional group and a hydrolytic group, the material treated by silane has good compatibility in an organic solvent and an aqueous solution, so that the silane can be used for improving the dispersion performance of inorganic powder in a coating. The silane structure contains one or more organic functional groups and hydrolytic groups, and the hydrolysis and polycondensation principles are shown in figure 1. As shown in FIG. 1, after the silane is hydrolyzed, a large number of silanol groups [ Si-OH ] can be generated, and the groups not only can be self-condensed, but also can generate cross-linking reaction with hydroxyl adsorbed on the surface of the powder particles, so that the surface of the particles is coated with a firmly-adhered and compact monomolecular layer silane film. Because the organic functional group in the silane structure has better compatibility with the organic solvent, the powder particles coated with the silane film are easy to disperse uniformly in the organic solvent and obtain higher stability. FIG. 2 shows a schematic diagram of the surface of the powder coated with a silane film. As can be readily understood from the schematic diagram of fig. 2, the aminosilane surface treatment greatly improves the storage stability of the fine powder particles in an organic solvent.
As a further improvement of the technical scheme of the preparation method, 10.0-20.0 parts of aminosilane is contained in the silane hydrolysis solution; 35.0-75.0 parts of absolute ethyl alcohol; 4.0 to 9.0 portions of deionized water.
As a further improvement of the technical scheme of the preparation method, the mass ratio of the silane hydrolysis solution to the mixed powder is 1: 1.
as a further improvement of the technical scheme of the preparation method, the aminosilane in the step (1) is gamma-aminopropyltriethoxysilane H2N-CH2CH2CH2-Si(OC2H5)3。
As a further improvement of the technical scheme of the preparation method, the stirring time in the step (4) is 12-48 h.
As a further improvement of the technical scheme of the preparation method, the ball milling time in the step (6) is 2-8 h.
As a further improvement of the technical scheme of the preparation method, the drying temperature of the powder slurry in the step (7) is 120 ℃.
Compared with the prior art, the silane modified high-temperature-resistant anti-oxidation coating material and the preparation method thereof have the beneficial effects that:
according to the silane modified high-temperature-resistant oxidation-resistant coating material, the metal oxide is used as the base material, and the aminosilane is used for treating the oxide powder, so that the oxide powder is more easily and uniformly dispersed in the coating and can stably exist, a foundation is laid for forming a uniform, compact and firmly-adhered coating, and the coating with an excellent protection effect is beneficial to improving the quality of hot-rolled steel. Therefore, the silane modified high-temperature-resistant anti-oxidation coating material and the preparation method thereof provided by the invention have good dispersibility and suspension stability, and can be used as a protective coating material for the hot rolling process of 9Ni steel.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of the hydrolysis and polycondensation principle of the silane structure.
FIG. 2 is a schematic diagram of a silane film coated on the surface of a powder. In the figure, Y is an organic functional group.
FIG. 3 shows that 100g of silane-modified high temperature-resistant and oxidation-resistant coating material prepared in example 3 of the present invention and 2.0 ml of non-silane-modified high temperature-resistant and oxidation-resistant coating material were added to 70ml of the mixturewthe t% propylene glycol aqueous solution is uniformly dispersed; a schematic diagram of the sedimentation of 10ml of the suspension after being taken out and allowed to stand at room temperature for 24 hours. In the figure, (a) unmodified coating material; (b) a modified coating material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
The technical solution of the present invention will be described in detail below with reference to the accompanying drawings.
The following examples demonstrate suspension stability performance: adding silane modified coating material to 2.0wtDispersing in% propylene glycol water solution for 30 min; standing the uniformly dispersed suspension for 24h at normal temperature, measuring the height of sediment at the bottom of the container, wherein the less the sediment is, the higher the suspension performance is.
The high-temperature resistant and oxidation resistant coating material which is not modified by silane is 2.0wt% CThe precipitation of the aqueous glycol solution after standing at room temperature for 24 hours is shown in FIG. 1.
The silane modified high temperature resistant oxidation resistant coating material prepared in the following example is added into 2.0wtThe% propylene glycol aqueous solution was dispersed for 30min and then allowed to stand at room temperature for 24 hours, and the sedimentation was shown in FIG. 2.
Example one
A silane modified high-temperature-resistant anti-oxidation coating material comprises the following components in parts by mass:
(1) nano SiO230.0 parts; (2) nano Al2O36.0 parts of (B); (3) 4.0 parts of nano MgO; (4) nano TiO 222.0 parts of (B); (5) 15.0 parts of SiC; (6) b is2O34.0 parts.
The silane modified high-temperature-resistant oxidation-resistant coating material prepared by the method provided by the invention comprises the following preparation steps:
a) preparing silane hydrolysis solution
The silane hydrolysis solution comprises the following components in parts by mass: 10.0 parts of aminosilane; 35.0 parts of absolute ethyl alcohol; 4.0 parts of deionized water.
(1) Weighing aminosilane, absolute ethyl alcohol and deionized water according to the mass ratio of the components of the silane hydrolysis solution;
(2) under the condition of continuous stirring, firstly, adding absolute ethyl alcohol into aminosilane, and then slowly dropwise adding deionized water into a mixed solution of silane and ethyl alcohol;
(3) adjusting the pH value of the mixed solution to 9.0-10.0 by using ammonia water;
(4) and (3) placing the mixed solution in a water bath at 40 ℃, and continuously stirring for 12h to obtain a silane hydrolysis solution.
b) Preparation of powder Material
(5) Weighing raw material powder according to the mass ratio of a silane modified high-temperature-resistant oxidation-resistant coating material, and uniformly stirring to obtain mixed powder;
(6) according to the mass ratio of 1: 1, adding a silane hydrolysis solution into the mixed powder, and then carrying out ball milling for 2 hours to obtain mixed powder slurry;
(7) drying the powder slurry at 120 ℃, and then cooling to room temperature to obtain dried mixed powder;
(8) and crushing the dried mixed powder, and then sieving for three times, wherein the size of a sieve pore is 100-200 meshes, so as to obtain the silane modified high-temperature-resistant anti-oxidation coating material powder.
Weighing 100g of silane modified high temperature resistant and oxidation resistant coating material powder, adding into 70ml of 2.0wtDispersing in% propylene glycol water solution for 30 min; taking out 10ml of suspension, and standing for 24 hours at normal temperature until no obvious sediment is found; under the same conditions, the coating material powder which was not modified with silane (step a was not performed), and the silane hydrolysis solution was not added in step (6) was added to the propylene glycol aqueous solution, and the height of the sediment was measured to be 3.2 cm.
In this example, the aminosilane used was gamma-aminopropyltriethoxysilane H2N-CH2CH2CH2-Si(OC2H5)3Otherwise, the same procedure as in example 1 was repeated.
Example two
A silane modified high-temperature-resistant anti-oxidation coating material comprises the following components in parts by mass:
(1) nano SiO235.0 parts of (B); (2) nano Al2O36.5 parts; (3) 5.0 parts of nano MgO; (4) nano TiO 223.0 parts of (B); (5) 18.0 parts of SiC; (6) b is2O34.5 parts.
The silane modified high-temperature-resistant oxidation-resistant coating material prepared by the method provided by the invention comprises the following preparation steps:
a) preparing silane hydrolysis solution
The silane hydrolysis solution comprises the following components in parts by mass: 14.0 parts of aminosilane; 45.0 parts of absolute ethyl alcohol; 6.0 parts of deionized water.
(1) Weighing aminosilane, absolute ethyl alcohol and deionized water according to the mass ratio of the components of the silane hydrolysis solution;
(2) under the condition of continuous stirring, firstly, adding absolute ethyl alcohol into aminosilane, and then slowly dropwise adding deionized water into a mixed solution of silane and ethyl alcohol;
(3) adjusting the pH value of the mixed solution to 9.0-10.0 by using ammonia water;
(4) and (3) placing the mixed solution in a water bath at 40 ℃, and continuously stirring for 24 hours to obtain a silane hydrolysis solution.
b) Preparation of powder Material
(5) Weighing raw material powder according to the mass ratio of a silane modified high-temperature-resistant oxidation-resistant coating material, and uniformly stirring to obtain mixed powder;
(6) according to the mass ratio of 1: 1, adding a silane hydrolysis solution into the mixed powder, and then carrying out ball milling for 4 hours to obtain mixed powder slurry;
(7) drying the powder slurry at 120 ℃, and then cooling to room temperature to obtain dried mixed powder;
(8) and crushing the dried mixed powder, and then sieving for three times, wherein the size of a sieve pore is 100-200 meshes, so as to obtain the silane modified high-temperature-resistant anti-oxidation coating material powder.
Weighing 100g of silane modified high temperature resistant and oxidation resistant coating material powder, adding into 70ml of 2.0wtDispersing in% propylene glycol water solution for 30 min; taking out 10ml of suspension, and standing for 24 hours at normal temperature until no obvious sediment is found; under the same conditions, the coating material powder which was not modified with silane (step a was not performed), and the silane hydrolysis solution was not added in step (6) was added to the propylene glycol aqueous solution, and the height of the sediment was measured to be 3.7 cm.
EXAMPLE III
A silane modified high-temperature-resistant anti-oxidation coating material comprises the following components in parts by mass:
(1) nano SiO240.0 parts; (2) nano Al2O37.0 parts; (3) 6.0 parts of nano MgO; (4) nano TiO 224.0 parts of (B); (5) 21.0 parts of SiC; (6) b is2O35.0 parts.
The silane modified high-temperature-resistant oxidation-resistant coating material prepared by the method provided by the invention comprises the following preparation steps:
a) preparing silane hydrolysis solution
The silane hydrolysis solution comprises the following components in parts by mass: 18.0 parts of aminosilane; 55.0 parts of absolute ethyl alcohol; 8.0 parts of deionized water.
(1) Weighing aminosilane, absolute ethyl alcohol and deionized water according to the mass ratio of the components of the silane hydrolysis solution;
(2) under the condition of continuous stirring, firstly, adding absolute ethyl alcohol into aminosilane, and then slowly dropwise adding deionized water into a mixed solution of silane and ethyl alcohol;
(3) adjusting the pH value of the mixed solution to 9.0-10.0 by using ammonia water;
(4) and (3) placing the mixed solution in a water bath at 40 ℃, and continuously stirring for 36 hours to obtain a silane hydrolysis solution.
b) Preparation of powder Material
(5) Weighing raw material powder according to the mass ratio of a silane modified high-temperature-resistant oxidation-resistant coating material, and uniformly stirring to obtain mixed powder;
(6) according to the mass ratio of 1: 1, adding a silane hydrolysis solution into the mixed powder, and then carrying out ball milling for 6 hours to obtain mixed powder slurry;
(7) drying the powder slurry at 120 ℃, and then cooling to room temperature to obtain dried mixed powder;
(8) and crushing the dried mixed powder, and then sieving for three times, wherein the size of a sieve pore is 100-200 meshes, so as to obtain the silane modified high-temperature-resistant anti-oxidation coating material powder.
Weighing 100g of silane modified high temperature resistant and oxidation resistant coating material powder, adding into 70ml of 2.0wtDispersing in% propylene glycol water solution for 30 min; taking out 10ml of suspension, and standing for 24 hours at normal temperature until no obvious sediment is found; under the same conditions, the coating material powder which was not modified with silane (step a was not performed), and the silane hydrolysis solution was not added in step (6) was added to the propylene glycol aqueous solution, and the height of the sediment was measured to be 4.0 cm.
Example four
A silane modified high-temperature-resistant anti-oxidation coating material comprises the following components in parts by mass:
(1) nano SiO2 50.0 part; (2) nano Al2O38.0 parts of (B); (3) 7.0 parts of nano MgO; (4) nano TiO 225.0 parts of (B); (5) 25.0 parts of SiC; (6) b is2O36.0 parts.
The silane modified high-temperature-resistant oxidation-resistant coating material prepared by the method provided by the invention comprises the following preparation steps:
a) preparing silane hydrolysis solution
The silane hydrolysis solution comprises the following components in parts by mass: 20.0 parts of aminosilane; 70.0 parts of absolute ethyl alcohol; and 9.0 parts of deionized water.
(1) Weighing aminosilane, absolute ethyl alcohol and deionized water according to the mass ratio of the components of the silane hydrolysis solution;
(2) under the condition of continuous stirring, firstly, adding absolute ethyl alcohol into aminosilane, and then slowly dropwise adding deionized water into a mixed solution of silane and ethyl alcohol;
(3) adjusting the pH value of the mixed solution to 9.0-10.0 by using ammonia water;
(4) and (3) placing the mixed solution in a water bath at 40 ℃, and continuously stirring for 48 hours to obtain a silane hydrolysis solution.
b) Preparation of powder Material
(5) Weighing raw material powder according to the mass ratio of a silane modified high-temperature-resistant oxidation-resistant coating material, and uniformly stirring to obtain mixed powder;
(6) according to the mass ratio of 1: 1, adding a silane hydrolysis solution into the mixed powder, and then carrying out ball milling for 8 hours to obtain mixed powder slurry;
(7) drying the powder slurry at 120 ℃, and then cooling to room temperature to obtain dried mixed powder;
(8) and crushing the dried mixed powder, and then sieving for three times, wherein the size of a sieve pore is 100-200 meshes, so as to obtain the silane modified high-temperature-resistant anti-oxidation coating material powder.
Weighing 100g of silane modified high temperature resistant and oxidation resistant coating material powder, adding into 70ml of 2.0wtDispersing in% propylene glycol water solution for 30 min; taking out 10ml of suspension, and standing for 24 hours at normal temperature until no obvious sediment is found; under the same conditions, doThe powder of the coating material modified with silane (not subjected to step a) and to which the silane hydrolysis solution was not added in step (6) was added to the propylene glycol aqueous solution, and the height of the sediment was measured to be 4.5 cm.
The silane modified high-temperature-resistant antioxidant coating material and the preparation method thereof can be applied to a surface protection process used in a 9Ni steel hot rolling process, powder of the coating material can be well dispersed and stabilized in an organic solvent, the sedimentation amount of the coating material is obviously lower than that of the coating material which is not modified by silane, a reliable base material is provided for preparing an excellent high-temperature-resistant antioxidant coating, and the problems of poor suspension stability and the like of the conventional high-temperature-resistant antioxidant coating are solved.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (6)
1. A preparation method of a silane modified high-temperature-resistant anti-oxidation coating material is characterized by comprising the following steps:
a) preparing silane hydrolysis solution
(1) Weighing gamma-aminopropyl triethoxysilane H2N-CH2CH2CH2-Si(OC2H5)3Absolute ethyl alcohol and deionized water;
(2) under the condition of continuous stirring, firstly, absolute ethyl alcohol is added into gamma-aminopropyl triethoxysilane H2N-CH2CH2CH2-Si(OC2H5)3Then slowly dropwise adding deionized water to the gamma-aminopropyl triethoxysilane H2N-CH2CH2CH2-Si(OC2H5)3And ethanol;
(3) adjusting the pH value of the mixed solution to 9.0-10.0 by using ammonia water;
(4) placing the mixed solution in a water bath at 40 ℃, and continuously stirring to obtain a silane hydrolysis solution;
b) preparation of powder Material
(5) Weighing raw material powder according to the mass parts of the components of the silane-modified high-temperature-resistant anti-oxidation coating material, and uniformly stirring to obtain mixed powder; the silane modified high-temperature-resistant anti-oxidation coating material is composed of the following components in parts by mass: nano SiO230.0 to 50.0 portions of nano Al2O36.0-8.0 parts of nano MgO 4.0-7.0 parts of nano TiO22.0-5.0 parts of silicon carbide SiC 15.0-25.0 parts of boron oxide B2O34.0-6.0 parts;
(6) adding a silane hydrolysis solution into the mixed powder, and then carrying out ball milling to obtain mixed powder slurry;
(7) drying the powder slurry, and then cooling to room temperature to obtain dried mixed powder;
(8) and crushing the dried mixed powder, and then sieving for three times to obtain silane modified high-temperature-resistant anti-oxidation coating material powder.
2. The method for preparing the silane modified high temperature resistant and oxidation resistant coating material according to claim 1, wherein in the silane hydrolysis solution, 10.0-20.0 parts of aminosilane; 35.0-75.0 parts of absolute ethyl alcohol; 4.0 to 9.0 portions of deionized water.
3. The preparation method of the silane-modified high-temperature-resistant and antioxidant coating material as claimed in claim 1, wherein the mass ratio of the silane hydrolysis solution to the mixed powder is 1: 1.
4. the preparation method of the silane-modified high temperature-resistant and oxidation-resistant coating material as claimed in claim 1, wherein the stirring time in the step (4) is 12-48 h.
5. The preparation method of the silane-modified high-temperature-resistant and oxidation-resistant coating material as claimed in claim 1, wherein the ball milling time in step (6) is 2-8 h.
6. The method for preparing the silane-modified high-temperature-resistant and antioxidant coating material as claimed in claim 1, wherein the drying temperature of the powder slurry in the step (7) is 120 ℃.
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