CN116463052B - Organosilicon anticorrosive paint - Google Patents
Organosilicon anticorrosive paint Download PDFInfo
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- CN116463052B CN116463052B CN202310316313.7A CN202310316313A CN116463052B CN 116463052 B CN116463052 B CN 116463052B CN 202310316313 A CN202310316313 A CN 202310316313A CN 116463052 B CN116463052 B CN 116463052B
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- 239000003973 paint Substances 0.000 title claims abstract description 31
- 239000002131 composite material Substances 0.000 claims abstract description 64
- 239000000945 filler Substances 0.000 claims abstract description 45
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 41
- 239000010703 silicon Substances 0.000 claims abstract description 41
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000007822 coupling agent Substances 0.000 claims abstract description 28
- 239000011159 matrix material Substances 0.000 claims abstract description 25
- 238000000576 coating method Methods 0.000 claims abstract description 21
- 239000011521 glass Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000011324 bead Substances 0.000 claims abstract description 16
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000010445 mica Substances 0.000 claims abstract description 16
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 15
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 14
- 229920005989 resin Polymers 0.000 claims abstract description 14
- 239000011347 resin Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000005260 corrosion Methods 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 239000007921 spray Substances 0.000 claims abstract description 4
- XPBBUZJBQWWFFJ-UHFFFAOYSA-N fluorosilane Chemical compound [SiH3]F XPBBUZJBQWWFFJ-UHFFFAOYSA-N 0.000 claims abstract 12
- 239000000049 pigment Substances 0.000 claims description 34
- 238000010992 reflux Methods 0.000 claims description 21
- 239000010936 titanium Substances 0.000 claims description 19
- 229910052719 titanium Inorganic materials 0.000 claims description 19
- 229910052782 aluminium Inorganic materials 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 13
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 13
- -1 titanium siloxane Chemical class 0.000 claims description 13
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 claims description 12
- 229910000165 zinc phosphate Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 210000003298 dental enamel Anatomy 0.000 claims description 8
- 239000003085 diluting agent Substances 0.000 claims description 8
- 229920001296 polysiloxane Polymers 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 7
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 7
- 239000008096 xylene Substances 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- 239000002562 thickening agent Substances 0.000 claims description 5
- 239000000440 bentonite Substances 0.000 claims description 4
- 229910000278 bentonite Inorganic materials 0.000 claims description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical group O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 3
- QTRSWYWKHYAKEO-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecyl-tris(1,1,2,2,2-pentafluoroethoxy)silane Chemical compound FC(F)(F)C(F)(F)O[Si](OC(F)(F)C(F)(F)F)(OC(F)(F)C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F QTRSWYWKHYAKEO-UHFFFAOYSA-N 0.000 claims description 2
- 125000006374 C2-C10 alkenyl group Chemical group 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- BPCXHCSZMTWUBW-UHFFFAOYSA-N triethoxy(1,1,2,2,3,3,4,4,5,5,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F BPCXHCSZMTWUBW-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 9
- 238000009413 insulation Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 2
- 230000002209 hydrophobic effect Effects 0.000 abstract description 2
- 239000005871 repellent Substances 0.000 abstract description 2
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 description 17
- 238000000034 method Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 229920002050 silicone resin Polymers 0.000 description 4
- 239000002966 varnish Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- ZTXONRUJVYXVTJ-UHFFFAOYSA-N chromium copper Chemical compound [Cr][Cu][Cr] ZTXONRUJVYXVTJ-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 229920006255 plastic film Polymers 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229940089951 perfluorooctyl triethoxysilane Drugs 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- AVYKQOAMZCAHRG-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F AVYKQOAMZCAHRG-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Abstract
The invention discloses an organic silicon anticorrosive paint, which comprises organic silicon resin and an auxiliary agent, wherein the auxiliary agent comprises an inorganic composite filler, the inorganic composite filler is prepared by reacting a composite filler matrix with a fluorosilane coupling agent, the composite filler matrix is a mixture of mica powder, talcum powder and hollow glass beads, and the feeding mass ratio of the mica powder to the talcum powder to the hollow glass beads is 1.5-3.0:1:1.5-3.0; the invention not only realizes the functions of hydrophobic and water-repellent (the contact angle with water is larger than 105 degrees) of the organic silicon anticorrosive paint, the heat conductivity coefficient of the coating is less than 0.10W/(m.k), the corrosion resistance (the salt spray resistance test can reach 3000 h), but also has excellent heat resistance and heat insulation performance, and breaks through the use limitation of the traditional organic silicon anticorrosive paint.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a high-temperature anti-corrosion coating, and specifically relates to an organosilicon anti-corrosion coating.
Background
With the continuous development of advanced technologies such as science and technology, especially national defense technology, people put forward higher and higher requirements on the performance and construction latitude of high-temperature resistant coatings, not only are the coatings required to have excellent heat resistance at high temperature, but also the coatings are required to be cured at room temperature and form films continuously above room temperature; therefore, silicone high temperature resistant coatings have been developed. The organosilicon high-temperature resistant coating is mainly applied to high-temperature corrosion prevention in the fields of steel, petrifaction and military industry, and has quick development in recent years due to market pulling. The organosilicon high-temperature resistant paint generally adopts organosilicon resin and modified organosilicon resin as base materials, and is matched with various high-temperature resistant Wen Yan fillers and low-melting glass powder. However, along with the requirements of industrial production safety, energy conservation and emission reduction, the flame retardance, heat resistance and heat insulation performance of the high-temperature-resistant coating need to be further improved, and the flame retardance, heat resistance and heat insulation performance of the traditional organic silicon or modified organic silicon coating are difficult to meet the technical requirements of increasingly higher markets.
Disclosure of Invention
The invention aims to overcome one or more defects in the prior art and provides an improved organic silicon anticorrosive paint which can have heat resistance, heat insulation performance, water repellency and water repellency.
In order to achieve the above purpose, the invention adopts the following technical scheme: the organic silicon anticorrosive paint comprises organic silicon resin and an auxiliary agent, wherein the auxiliary agent comprises an inorganic composite filler, the inorganic composite filler is prepared by reacting a composite filler matrix with a fluorosilane coupling agent, the composite filler matrix is a mixture of mica powder, talcum powder and hollow glass beads, and the feeding mass ratio of the mica powder to the talcum powder to the hollow glass beads is 1.5-3.0:1:1.5-3.0;
The particle size of the mica powder is 700-900 meshes; the particle size of the talcum powder is 700-900 meshes; the particle size of the hollow glass beads is 5-60 mu m.
According to some preferred aspects of the invention, the auxiliary agent further comprises an inorganic composite pigment, wherein the inorganic composite pigment is prepared by reacting a pigment matrix with a fluorosilane coupling agent, the pigment matrix is a mixture of chrome-copper black and enamel black, and the feeding mass ratio of the chrome-copper black to the enamel black is 1.0-3.0:1. The inorganic composite pigment is matched with inorganic composite filler, and the hydrophobic and water-repellent functions of the whole material can be further increased on the basis of the basic filler function.
According to some preferred aspects of the invention, the fluorosilane coupling agent comprises at least one of perfluorooctyl triethoxysilane, tridecafluorooctyl triethoxysilane, perfluorodecyl triethoxysilane.
According to some preferred aspects of the present invention, the fluorosilane coupling agent is added in an amount of 3% to 20%, preferably 5% to 15% by mass of the composite filler matrix.
According to some preferred aspects of the present invention, the fluorosilane coupling agent is added in an amount of 3% to 20%, preferably 5% to 15%, of the pigment base.
According to some preferred and specific aspects of the invention, embodiments of preparing the inorganic composite filler include: adding the dried composite filler matrix, the fluorosilane coupling agent and the reflux xylene into a container with stirring paddles and a reflux condenser, heating to 80-90 ℃, dropwise adding the catalyst trifluoroacetic acid with a formula amount, heating to 110-125 ℃ for reflux reaction, filtering, removing the solvent and the excessive fluorosilane coupling agent which is not grafted, and drying in a drying oven to obtain the inorganic composite filler.
According to some preferred and specific aspects of the present invention, embodiments for preparing the inorganic composite pigment include: adding the dried pigment matrix, the fluorosilane coupling agent and the reflux xylene into a container with stirring paddles and a reflux condenser, heating to 80-90 ℃, dripping the catalyst trifluoroacetic acid with the formula amount, heating to 110-125 ℃ for reflux reaction, filtering, removing the solvent and the excessive fluorosilane coupling agent which is not grafted, and drying in a drying oven to obtain the inorganic composite pigment.
According to some preferred aspects of the present invention, the inorganic composite filler is added in an amount of 3% -15% by mass of the raw material.
According to some preferred aspects of the present invention, the inorganic composite pigment is added in an amount of 10% to 25% by mass of the raw material.
According to some preferred aspects of the present invention, the inorganic composite pigment is added in an amount of 1.5 to 3.5 times the amount of the inorganic composite filler.
According to some preferred aspects of the invention, the auxiliary agent further comprises aluminum and/or zinc phosphate, and compared with other materials, the antirust performance of the anticorrosive paint can be remarkably improved.
According to some preferred aspects of the invention, the aluminum and/or zinc phosphate is composed of aluminum tripolyphosphate and zinc phosphate, and the feeding mass ratio of the aluminum tripolyphosphate to the zinc phosphate is 0.3-0.8:1.
According to some preferred aspects of the invention, the aluminum and/or zinc phosphate is added in an amount of 4% -20% by mass of the raw material.
According to some preferred aspects of the invention, the adjuvant further comprises a thickener which is bentonite.
According to some preferred aspects of the present invention, the thickener is added in an amount of 0.001% -1% by mass of the raw material.
According to some preferred aspects of the invention, the auxiliary agent further comprises a diluent, wherein the diluent comprises propylene glycol methyl ether acetate, and the addition amount of the diluent is 6-20% of the raw materials in percentage by mass.
According to some preferred aspects of the invention, the silicone resin contains a silanol group as a terminal group;
The raw materials also comprise nano titanium dioxide hybridized polyaluminium titanium siloxane shown in the following formula;
wherein each X 1、X2、X3、X4、X5 is independently selected from the group consisting of:
And X 1、X2、X3、X4、X5 has terminal hydroxyl groups, any two of which are not repeated and at least comprise One of them;
t1, t2, t3, t4, t5 are independently selected from 0 to 100 and are not 0 when the corresponding group contains aluminum or titanium;
R 1、R2、R3、R4、R5、R6、R7、R8、R9 is independently selected from C 1-20 alkyl, phenyl, C 1-6 alkyl substituted phenyl, C 2-10 alkenyl;
M is titanium dioxide, which is connected with silicon hydroxyl, aluminum hydroxyl or titanium hydroxyl through hydrogen bond through hydroxyl contained on the surface;
The mass ratio of the nano titanium dioxide hybridized polyaluminium titanium siloxane to the organic silicon resin is 0.3-0.5:1.
In the present invention, the presence of a terminal hydroxyl group in X 1、X2、X3、X4、X5 may mean that a silicon hydroxyl group, an aluminum hydroxyl group, a titanium hydroxyl group, or the like is present on the segment structure, or may mean that a hydroxyl group is present on the surface of nano titanium dioxide.
According to some preferred aspects of the invention, wherein t1, t2, t3, t4, t5 are independently selected from 0-50, further 0-30, still further 0-20. In some embodiments of the invention, t1, t2, t3, t4, t5 are independently selected from 0, 1,2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20.
According to some preferred aspects of the invention, wherein R 1、R2、R3、R4、R5、R6、R7、R8、R9 is each independently selected from methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, n-pentyl, isopentyl, neopentyl, n-hexyl, phenyl, C 1-6 alkyl substituted phenyl, vinyl, methylvinyl, ethylvinyl, propylvinyl.
According to some preferred aspects of the present invention, the nano-titania hybrid polyaluminosiloxane has an average molecular weight of 500 to 10000, further 800 to 8000, still further 1000 to 5000. In some embodiments of the invention, the nano-titania hybrid polyaluminosiloxane has an average molecular weight of from 1500 to 4500.
According to the invention, the nano titanium dioxide hybrid polyaluminium titanium siloxanes of the invention can be in a highly viscous liquid or paste form.
According to some preferred aspects of the invention, the method for preparing the organosilicon anticorrosive paint comprises the following steps: reflux-reacting nano titanium dioxide hybridized polyaluminium-titanium siloxane, organic silicon resin containing silicon hydroxyl and a first solvent at 130-160 ℃, evaporating the first solvent after the reaction is finished and reacting to generate low molecular substances, adding an auxiliary agent, and uniformly mixing to prepare the organic silicon anticorrosive paint.
In the present invention, the silicone resin containing a silicon hydroxyl group is commercially available, and for example, silicone resin 9802R may be used.
In some embodiments of the invention, embodiments of preparing the silicone anticorrosive coating include: ① Adding nano titanium dioxide hybridized polyaluminium-titanium siloxane, organic silicon resin containing silicon hydroxyl and refluxing xylene into a container provided with a stirring paddle and a reflux condenser, carrying out reflux reaction at 135-145 ℃, cooling, distilling off xylene under vacuum and low molecular substances generated by the reaction, cooling to room temperature, and adding a diluent; ② Adding the product ① and aluminum tripolyphosphate, zinc phosphate and bentonite into a dispersing cylinder, and stirring to obtain a uniform premix; then adding inorganic composite filler and inorganic composite pigment, continuously stirring, and controlling the temperature of a dispersing cylinder to be less than or equal to 55 ℃ during stirring to prepare the organosilicon anti-corrosive paint.
According to the invention, the grafting of the nano titanium dioxide hybridized polyaluminium titanium siloxane into the molecular structure of the organic silicon resin is realized through condensation of the nano titanium dioxide hybridized polyaluminium titanium siloxane and the surface silicon hydroxyl and/or the titanium hydroxyl and the organic silicon resin containing the silicon hydroxyl, and excellent flame retardant property and high temperature resistance are provided for the organic silicon resin on the basis of realizing excellent dispersing effect.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
The inventor has unexpectedly found that after the specific inorganic filler is adopted to combine and carry out the fluorine-silicon surface modification, the organic silicon anticorrosive paint has the functions of hydrophobicity and water repellency (the contact angle with water is larger than 105 degrees), the heat conductivity coefficient of the coating is less than 0.10W/(m.k), the corrosion resistance (the salt spray resistance test can reach 3000 h), the excellent heat resistance and the heat insulation performance are also achieved, and the use limitation of the traditional organic silicon anticorrosive paint is broken through.
Detailed Description
The above-described aspects are further described below in conjunction with specific embodiments; it should be understood that these embodiments are provided to illustrate the basic principles, main features and advantages of the present invention, and that the present invention is not limited by the scope of the following embodiments; the implementation conditions employed in the examples may be further adjusted according to specific requirements, and the implementation conditions not specified are generally those in routine experiments.
All starting materials are commercially available or prepared by methods conventional in the art, not specifically described in the examples below.
The nano-titania hybrid polyaluminium titanium siloxanes M used in the examples below were prepared by the method of example 9 of patent CN 2022114767155.
The nano titanium dioxide hybrid polyaluminium titanium siloxane N used in the following examples was prepared by the method of example 8 in patent CN 2022114767155.
Silicone resin 9802R was purchased from carnot silicone limited, inc; aluminum tripolyphosphate, available from Guangxi-province institute of functional materials, trade name AP-30; zinc phosphate, available from Guangxi Productivity institute of functional materials, brand ZP-50; mica powder, available from Guangdong source epitaxial powder Co., ltd., brand coating grade, 800 mesh; talcum powder, available from Guangdong source epitaxial powder Co., ltd., brand coating grade, 800 mesh; hollow glass beads, available from Guangdong Megaotong glass plastic technology Co., ltd., brand 3010, parameter particle size range 10-45 μm; chrome copper black NL-04, available from Hunan Norrisi New Material Co., ltd., brand NL-04; enamel black, available from Hunan Norrisi New Material Co., ltd., brand NL-11.
Examples 1 to 6
The raw material formulas of the organic silicon anticorrosive paint are shown in table 1.
TABLE 1
Wherein the inorganic composite filler is prepared by reacting a composite filler matrix with a fluorosilane coupling agent, the composite filler matrix is a mixture of mica powder, talcum powder and hollow glass beads (the mass ratio of the mica powder to the talcum powder to the hollow glass beads is 2:1:2), and the formula raw materials of the fluorosilicone surface modified composite filler A, the fluorosilicone surface modified composite filler B and the fluorosilicone surface modified composite filler C are shown in the table 2;
TABLE 2
The preparation method of the inorganic composite filler comprises the following steps: adding 50g of composite filler matrix (wherein, 20g of mica powder, 10g of talcum powder and 20g of hollow glass beads) which are dried for 24 hours under vacuum at 180 ℃ and fluorosilane coupling agent which accounts for about 10 percent of the mass of the composite filler and dimethylbenzene which is 15 times of the dosage of the composite filler matrix into a 1000mL three-neck flask which is provided with a stirring paddle and a reflux condenser, heating to about 85 ℃, dropwise adding the catalyst trifluoroacetic acid with the formula dosage within 30min, and heating to 115 ℃ for reflux reaction for more than 4 hours. And then filtering, removing the solvent and the excessive ungrafted fluorosilane coupling agent, drying for 2 hours in a vacuum oven at 120 ℃, and sealing for recycling to obtain the inorganic composite filler.
The inorganic composite pigment is prepared by reacting a pigment matrix with a fluorosilane coupling agent, wherein the pigment matrix is a mixture of chromium copper black and enamel black, the feeding mass ratio of the chromium copper black NL-04 to the enamel black NL-11 is 2:1, and the formula raw materials of the fluorosilicone surface modified composite pigment I, the fluorosilicone surface modified composite pigment II and the fluorosilicone surface modified composite pigment III are shown in the table 3;
TABLE 3 Table 3
The preparation method of the inorganic composite pigment comprises the following steps: a500 mL three-necked flask equipped with a stirring paddle and a reflux condenser was charged with 30g of a pigment base body dried under vacuum at 180℃for 24 hours (wherein: 20g of chrome copper black (NL-04), 10g of enamel black (NL-11)), about 10% by mass of a fluorosilane coupling agent and 10 times by mass of xylene as much as the pigment base body, and the temperature was raised to about 85℃and a prescribed amount of trifluoroacetic acid as a catalyst was added dropwise within 30 minutes, and the reflux reaction was carried out at 115℃for 4 hours or more. And then filtering, removing the solvent and the excessive ungrafted fluorosilane coupling agent, drying for 2 hours in a vacuum oven at 120 ℃, and sealing for recycling to obtain the inorganic composite pigment.
The preparation method of the organic silicon anticorrosive paint comprises the following steps: ① Adding nano titanium dioxide hybridized polyaluminium titanium siloxane, organic silicon resin 9802R and dimethylbenzene with the formula amount in table 1 into a four-neck flask with stirring paddles and a reflux condenser, carrying out reflux reaction for 60min at 140 ℃, reducing the temperature to 100+/-5 ℃ and reducing the pressure to distill dimethylbenzene and low molecular substances generated by the reaction under the vacuum degree of 0.095MPa, reducing the temperature to room temperature, and adding the diluent (propylene glycol methyl ether acetate) with the formula amount in table 1; ② Adding ① of the product and the auxiliary agents (aluminum tripolyphosphate, zinc phosphate and bentonite) with the formula amount shown in table 1 into a dispersing cylinder, stirring at the stirring speed of 400 rpm for 30 minutes to obtain a uniform premix; then adding the inorganic composite pigment and the inorganic composite filler in the table 1, continuously stirring and dispersing for 30 minutes at the stirring speed of 600 revolutions per minute, and controlling the temperature of a dispersing cylinder to be less than or equal to 55 ℃ during the period, so as to prepare the organosilicon anti-corrosive paint.
Comparative example 1
Substantially the same as in example 1, the only difference is that: the mica powder, talcum powder and hollow glass beads in the inorganic composite filler are not modified by the fluorosilane coupling agent.
Comparative example 2
Substantially the same as in example 1, the only difference is that: mica powder, talcum powder 20g and hollow glass beads 30g are not added into the raw materials of the inorganic composite filler.
Comparative example 3
Substantially the same as in example 1, the only difference is that: talcum powder, mica powder 25g and hollow glass beads 25g are not added into the raw materials of the inorganic composite filler.
Comparative example 4
Substantially the same as in example 1, the only difference is that: hollow glass beads, 30g of mica powder and 20g of talcum powder are not added into the raw materials of the inorganic composite filler.
Performance testing
The silicone anticorrosive coatings obtained in examples 1 to 6 and comparative examples 1 to 4 were subjected to the following performance tests, and specific results are shown in table 4.
TABLE 4 Table 4
Test standard:
heat resistance (c): GB/T1735-2009 determination of heat resistance of paints and varnishes;
Contact angle with water degree: GB/T30693-2014 measurement of contact angle of Plastic film with Water;
limiting oxygen index%: GB/T2406.2-2009 section 2 for determination of Combustion behavior by oxygen index method for plastics: room temperature test;
Adhesion (steel)/MPa: GB/T5210-2006, adhesion test of paint and varnish pull-off method;
salt spray resistance (3000 h): GB/T2423.17-2008 "Electrical and electronic product Environment test section 2 test method test Ka: salt fog
A liquid medium (30 d) resistant to 10% hcl: GB/T30648.1-2014 determination of liquid resistance of paints and varnishes part 1: immersed in a liquid other than water;
Pencil hardness: GB/T6739-2006 "determination of paint film hardness by the paint and varnish Pencil method";
Impact strength (J/m 2): GB/T8809-2015 method for testing plastic film against pendulum impact;
thermal conductivity W/(m·k): GB/T10295-2008 "measurement of thermal resistance of insulation Material in steady state (Heat flow Meter method)" and related Properties.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
Claims (10)
1. The organic silicon anticorrosive paint is characterized in that the auxiliary agent comprises inorganic composite filler and inorganic composite pigment, wherein the inorganic composite filler is prepared by reacting a composite filler matrix with a fluorosilane coupling agent, the composite filler matrix is a mixture of mica powder, talcum powder and hollow glass beads, and the feeding mass ratio of the mica powder to the talcum powder to the hollow glass beads is 1.5-3.0:1:1.5-3.0;
the particle size of the mica powder is 700-900 meshes; the particle size of the talcum powder is 700-900 meshes; the particle size of the hollow glass beads is 5-60 mu m;
The inorganic composite pigment is prepared by reacting a pigment matrix with a fluorosilane coupling agent, wherein the pigment matrix is a mixture of chrome-copper black and enamel black, and the feeding mass ratio of the chrome-copper black to the enamel black is 1.0-3.0:1;
The addition amount of the inorganic composite pigment is 1.5-3.5 times of the addition amount of the inorganic composite filler;
The organic silicon resin contains silicon hydroxyl as a terminal group;
The raw materials also comprise nano titanium dioxide hybridized polyaluminium titanium siloxane shown in the following formula;
wherein each X 1、X2、X3、X4、X5 is independently selected from the group consisting of: And X 1、X2、X3、X4、X5 has terminal hydroxyl groups, any two of which are not repeated and at least comprise One of them;
t1, t2, t3, t4, t5 are independently selected from 0 to 100 and are not 0 when the corresponding group contains aluminum or titanium;
R 1、R2、R3、R4、R5、R6、R7、R8、R9 is independently selected from C 1-20 alkyl, phenyl, C 1-6 alkyl substituted phenyl, C 2-10 alkenyl;
M is titanium dioxide, which is connected with silicon hydroxyl, aluminum hydroxyl or titanium hydroxyl through hydrogen bond through hydroxyl contained on the surface;
The feeding mass ratio of the nano titanium dioxide hybridized polyaluminium titanium siloxane to the organic silicon resin is 0.3-0.5:1;
The contact angle between the organosilicon anti-corrosion coating and water is more than 105 degrees, the heat conductivity coefficient of the coating is less than 0.10W/(m.k), and the salt spray resistance can reach 3000 hours.
2. The silicone anticorrosive coating according to claim 1, wherein the fluorosilane coupling agent comprises at least one of tridecafluorooctyltriethoxysilane, perfluorodecyltriethoxysilane.
3. The organic silicon anticorrosive paint according to claim 1, wherein the addition amount of the fluorosilane coupling agent is 3% -20% of the addition amount of the composite filler matrix in mass percent;
The addition amount of the fluorosilane coupling agent is 3-20% of the addition amount of the pigment matrix in percentage by mass;
Embodiments for preparing the inorganic composite filler include: adding a dried composite filler matrix, a fluorosilane coupling agent and refluxing xylene into a container provided with a stirring paddle and a reflux condenser, heating to 80-90 ℃, dropwise adding a catalyst trifluoroacetic acid with a formula amount, heating to 110-125 ℃ for reflux reaction, filtering, removing a solvent and redundant fluorosilane coupling agent which is not grafted, and drying in a drying oven to obtain an inorganic composite filler;
Embodiments for preparing the inorganic composite pigment include: adding the dried pigment matrix, the fluorosilane coupling agent and the reflux xylene into a container with stirring paddles and a reflux condenser, heating to 80-90 ℃, dripping the catalyst trifluoroacetic acid with the formula amount, heating to 110-125 ℃ for reflux reaction, filtering, removing the solvent and the excessive fluorosilane coupling agent which is not grafted, and drying in a drying oven to obtain the inorganic composite pigment.
4. The organic silicon anticorrosive paint according to claim 3, wherein the addition amount of the fluorosilane coupling agent is 5% -15% of the addition amount of the composite filler matrix in mass percent;
the addition amount of the fluorosilane coupling agent is 5-15% of the addition amount of the pigment matrix in percentage by mass.
5. The organic silicon anticorrosive paint according to claim 1, wherein the inorganic composite filler is added in an amount of 3-15% of the raw material and the inorganic composite pigment is added in an amount of 10-25% of the raw material in terms of mass percent.
6. The silicone anticorrosive coating according to claim 1, wherein the auxiliary agent further comprises aluminum and/or zinc phosphate.
7. The organic silicon anticorrosive paint according to claim 6, wherein the phosphate of aluminum and/or zinc consists of aluminum tripolyphosphate and zinc phosphate, and the feeding mass ratio of the aluminum tripolyphosphate to the zinc phosphate is 0.3-0.8:1.
8. The organosilicon anticorrosive coating according to claim 6, wherein the amount of the aluminum and/or zinc phosphate added is 4-20% by mass of the raw material.
9. The organic silicon anticorrosive paint according to claim 1, wherein the auxiliary agent further comprises a thickening agent, wherein the thickening agent is bentonite, and the addition amount of the thickening agent is 0.001% -1% of the raw materials in terms of mass percent;
The auxiliary agent also comprises a diluent, wherein the diluent comprises propylene glycol methyl ether acetate, and the addition amount of the diluent accounts for 6-20% of the raw materials in percentage by mass.
10. The silicone anticorrosive paint according to claim 1, wherein the preparation method of the silicone anticorrosive paint comprises:
Reflux-reacting nano titanium dioxide hybridized polyaluminium-titanium siloxane, organic silicon resin containing silicon hydroxyl and a first solvent at 130-160 ℃, evaporating the first solvent after the reaction is finished and reacting to generate low molecular substances, adding an auxiliary agent, and uniformly mixing to prepare the organic silicon anticorrosive paint.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310316313.7A CN116463052B (en) | 2023-03-29 | Organosilicon anticorrosive paint |
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| CN202310316313.7A CN116463052B (en) | 2023-03-29 | Organosilicon anticorrosive paint |
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| CN110776788A (en) * | 2018-07-31 | 2020-02-11 | 宁波其兰文化发展有限公司 | Heat-insulation self-cleaning hybrid coating and preparation method thereof |
| CN110804393A (en) * | 2019-12-12 | 2020-02-18 | 西北永新涂料有限公司 | Preparation method of high-temperature-resistant coating with self-cleaning performance |
| CN115746306A (en) * | 2022-11-23 | 2023-03-07 | 武汉鼎业环保工程技术有限公司 | Modified polysiloxane and preparation method thereof |
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| CN102585696A (en) * | 2012-02-13 | 2012-07-18 | 江苏大学 | Methyl phenyl silicone resin base high-temperature-resistant coating and preparation method thereof |
| CN110776788A (en) * | 2018-07-31 | 2020-02-11 | 宁波其兰文化发展有限公司 | Heat-insulation self-cleaning hybrid coating and preparation method thereof |
| CN110804393A (en) * | 2019-12-12 | 2020-02-18 | 西北永新涂料有限公司 | Preparation method of high-temperature-resistant coating with self-cleaning performance |
| CN115746306A (en) * | 2022-11-23 | 2023-03-07 | 武汉鼎业环保工程技术有限公司 | Modified polysiloxane and preparation method thereof |
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