CN109504283B - Organosilicon coating with rigid molecular structure - Google Patents
Organosilicon coating with rigid molecular structure Download PDFInfo
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- CN109504283B CN109504283B CN201811327247.9A CN201811327247A CN109504283B CN 109504283 B CN109504283 B CN 109504283B CN 201811327247 A CN201811327247 A CN 201811327247A CN 109504283 B CN109504283 B CN 109504283B
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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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/10—Block or graft copolymers containing polysiloxane sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/442—Block-or graft-polymers containing polysiloxane sequences containing vinyl polymer sequences
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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
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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
- C09D5/18—Fireproof paints including high temperature resistant paints
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Abstract
An organosilicon coating with a rigid molecular structure is composed of 35-45% of aminoethyl aminopropyl polydimethylsiloxane, 5-10% of styrene maleic anhydride copolymer, 20-30% of mixed filler and 25-30% of cyclohexanone. The coating is used in a high-temperature corrosion environment, has good adhesive force to a base material, is easy to cure, can also ensure certain hardness and good flexibility, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of organic polymer coatings, in particular to an organic silicon coating with a rigid molecular structure.
Background
With the use of sophisticated automation and artificial exhaust equipment, smoke windows, stoves, heaters, incinerators, heat resistant coatings are gaining favor, and the development of the military industry places more stringent demands on the high temperature and corrosion resistance of coatings. The organosilicon polymer is composed of Si-O-Si chain links with the bond energy up to 441.3 kJ.mol-1The silicon-oxygen bond of the main chain is rarely damaged at high temperature, and the heat resistance of the single organic silicon polymer can reach 250 ℃, so that the organic silicon polymer has higher heat stability. In addition, silicone polymers have many other unique properties, such as corrosion resistance, weather resistance, low viscosity, low surface energy, etc., so their use in high temperature and corrosion resistant coatings has attracted considerable attention. However, the use of silicone polymers as coatings is also limited by problems such as poor adhesion to the substrate, difficulty in curing, residual flexibility and insufficient hardness. In response to the above problems, researchers have conducted many studies, mainly focusing on the polymerization of siliconesChemical modification of the product, and the like. Patents such as "a modified epoxy silicone coating (CN100584911C) resistant to high temperature and corrosion", "a modified silicone coating (CN 101113291A)", "a method of dip-coating a metal rubber article with a high temperature resistant silicone coating (CN 101733239A)" are silicone coatings prepared by utilizing the high temperature resistance of a silicone polymer while addressing the drawbacks of the silicone polymer when used alone. According to patent CN100584911C, the coating still has good salt fog corrosion resistance after high temperature, but the curing of the coating is mainly carried out by physical drying of the coating system, needs to be carried out at 250 ℃, and is long in time and difficult to cure. According to patent CN101113291A, the modified organosilicon coating has excellent corrosion resistance, high adhesion and high hardness, but the coating system is actually physical blending of organosilicon and epoxy resin, the compatibility of the coating system is poor, the coating is easy to generate phase separation phenomenon in the curing process, and the heat resistance, adhesion and the like of the coating are difficult to be ensured. According to patent CN101733239A, a film-forming substance of the coating is actually composed of epoxy organic silicon and a polyamide curing agent, and an epoxy structure and the polyamide curing agent in a coating system are cracked at a lower temperature in a high-temperature environment, so that the coating is difficult to have high temperature resistance.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide the organic silicon coating which is used in a high-temperature corrosion environment, has good adhesive force to a base material, is easy to cure, can simultaneously ensure certain hardness and good flexibility and has a rigid molecular structure, aiming at the defects that the existing high-temperature corrosion resistant organic silicon coating has poor adhesive force to the base material, is difficult to cure and is difficult to have flexibility and hardness at the same time.
The technical scheme is as follows: in order to achieve the purpose, the invention prepares the organic silicon coating with the rigid molecular structure by selecting the aminoethyl aminopropyl polydimethylsiloxane as a main film forming substance, taking the styrene maleic anhydride copolymer as a curing agent, taking a mixture of metal and inorganic filler as filler and taking cyclohexanone as a solvent. After the paint is coated on a metal substrate, a main film-forming substance and a curing agent are subjected to chemical reaction. The reaction of the aminoethyl aminopropyl polydimethylsiloxane and the styrene maleic anhydride copolymer is carried out in two steps, wherein in the first step, the acid anhydride in the molecular structure of the styrene maleic anhydride copolymer is subjected to ring opening at about 80 ℃ to generate a polyamic acid structure. The reaction equation involved is as follows:
the second step is that the polyamic acid structure obtained in the reaction is imidized at 160 ℃ to prepare the aminoethyl aminopropyl polydimethylsiloxane coating containing the rigid imide structure. The reaction equation involved is as follows:
the organic silicon coating with the rigid molecular structure comprises, by mass, 35-45% of aminoethyl aminopropyl polydimethylsiloxane, 5-10% of styrene maleic anhydride copolymer, 20-30% of mixed filler and 25-30% of cyclohexanone.
Preferably, the styrene maleic anhydride copolymer is in the form of powder, and has an acid value of 355, a number average molecular weight of 3000 and a weight average molecular weight of 750.
The preferable mixed filler is composed of aluminum powder, ferrophosphorus powder, mica powder and talcum powder according to the mass ratio of 1:2:6: 5.
The preparation method comprises the following steps: dissolving the aminoethyl aminopropyl polydimethylsiloxane into cyclohexanone, adding a mixed filler into a system, dispersing and mixing uniformly, and grinding the mixture to be less than 10 microns by using a grinder. And (3) uniformly mixing the mixture obtained by grinding with a styrene maleic anhydride copolymer, coating the mixture on a metal substrate, and heating the metal substrate at the temperature of 160 ℃ for 30 minutes to obtain the organosilicon coating with a rigid molecular structure.
Has the advantages that: the invention uses the aminoethyl aminopropyl polydimethylsiloxane as a main film forming substance, and the styrene maleic anhydride copolymer as a curing agent to obtain a coating which has good high-temperature corrosion resistance at first, and the reason is that the organic phase of the coating is the aminoethyl aminopropyl polydimethylsiloxane which has excellent temperature resistance, the rigid imide molecular structure in the system after the coating is cured also has excellent temperature resistance, and the organic silicon molecular structure has strong hydrophobicity, so the coating also has excellent corrosion resistance; secondly, because the coating contains amino, unreacted carboxyl, hydroxyl and other groups, the coating has good adhesive force to the metal base material, and meanwhile, the curing of the coating is easy to see from the technical scheme; most importantly, the siloxane bond in the molecular structure of the aminoethyl aminopropyl polydimethylsiloxane has excellent flexibility, so that the system simultaneously has a main chain structure with better flexibility and an imide side chain structure with higher rigidity, the combination of soft and hard sections on the molecular size of the coating is realized, and the coating simultaneously has certain hardness and good flexibility. The long-term use temperature of the coating is above 420 ℃, the salt spray resistance of the coating after high temperature (according to GB/T1771-2007) is not less than 10 days, the adhesive force (according to GB/1720-89) is more than one grade, the curing temperature is not more than 160 ℃, the curing time is not more than 1H, the hardness (according to GB/T6739-2006) is more than 4H, and the flexibility (according to GB/T1731 and 1993) of the coating is not more than 4 mm.
Detailed Description
Example 1:
the organic silicon coating with the rigid molecular structure is prepared from the following raw materials in percentage by mass:
dissolving aminoethyl aminopropyl polydimethylsiloxane into cyclohexanone, adding a mixed filler consisting of aluminum powder, ferrophosphorus powder, mica powder and talcum powder into a system, dispersing and mixing uniformly, and grinding the mixture to be less than 10 microns by using a grinder. And (3) uniformly mixing the mixture obtained by grinding with a styrene maleic anhydride copolymer, coating the mixture on a metal substrate, and heating the metal substrate at the temperature of 160 ℃ for 30 minutes to obtain the organosilicon coating with a rigid molecular structure. The long-term service temperature of the coating is 420 ℃, the salt spray resistance of the coating after high temperature (according to GB/T1771-2007) is 10 days, the adhesive force (according to GB/1720-89) is first grade, the curing temperature is not more than 160 ℃, the curing time is not more than 1H, the hardness (according to GB/T6739-2006) is 4H, and the flexibility (according to GB/T1731-1993) of the coating is 3 mm.
Example 2:
the organic silicon coating with the rigid molecular structure is prepared from the following raw materials in percentage by mass:
dissolving aminoethyl aminopropyl polydimethylsiloxane into cyclohexanone, adding a mixed filler consisting of aluminum powder, ferrophosphorus powder, mica powder and talcum powder into a system, dispersing and mixing uniformly, and grinding the mixture to be less than 10 microns by using a grinder. And (3) uniformly mixing the mixture obtained by grinding with a styrene maleic anhydride copolymer, coating the mixture on a metal substrate, and heating the metal substrate at the temperature of 160 ℃ for 30 minutes to obtain the organosilicon coating with a rigid molecular structure. The long-term service temperature of the coating is more than 430 ℃, the salt spray resistance of the coating after high temperature (according to GB/T1771-2007) is 11 days, the adhesive force (according to GB/1720-89) is first grade, the curing temperature is not more than 160 ℃, the curing time is not more than 1H, the hardness (according to GB/T6739-2006) is 4H, and the flexibility (according to GB/T1731 and 1993) of the coating is 4 mm.
Example 3:
the organic silicon coating with the rigid molecular structure is prepared from the following raw materials in percentage by mass:
dissolving aminoethyl aminopropyl polydimethylsiloxane into cyclohexanone, adding a mixed filler consisting of aluminum powder, ferrophosphorus powder, mica powder and talcum powder into a system, dispersing and mixing uniformly, and grinding the mixture to be less than 10 microns by using a grinder. And (3) uniformly mixing the mixture obtained by grinding with a styrene maleic anhydride copolymer, coating the mixture on a metal substrate, and heating the metal substrate at the temperature of 160 ℃ for 30 minutes to obtain the organosilicon coating with a rigid molecular structure. The long-term service temperature of the coating is more than 440 ℃, the salt spray resistance of the coating after high temperature (according to GB/T1771-2007) is 12 days, the adhesion (according to GB/1720-89) is 0 grade, the curing temperature is not more than 160 ℃, the curing time is not more than 1H, the hardness (according to GB/T6739-2006) is 5H, and the flexibility (according to GB/T1731 and 1993) of the coating is 4 mm.
Example 4:
the organic silicon coating with the rigid molecular structure is prepared from the following raw materials in percentage by mass:
dissolving aminoethyl aminopropyl polydimethylsiloxane into cyclohexanone, adding a mixed filler consisting of aluminum powder, ferrophosphorus powder, mica powder and talcum powder into a system, dispersing and mixing uniformly, and grinding the mixture to be less than 10 microns by using a grinder. And (3) uniformly mixing the mixture obtained by grinding with a styrene maleic anhydride copolymer, coating the mixture on a metal substrate, and heating the metal substrate at the temperature of 160 ℃ for 30 minutes to obtain the organosilicon coating with a rigid molecular structure. The long-term service temperature of the coating is 440 ℃, the salt spray resistance of the coating after high temperature (according to GB/T1771-2007) is 11 days, the adhesive force (according to GB/1720-89) is first grade, the curing temperature is not more than 160 ℃, the curing time is not more than 1H, the hardness (according to GB/T6739-2006) is 4H, and the flexibility (according to GB/T1731-1993) of the coating is 3 mm.
Example 5:
the organic silicon coating with the rigid molecular structure is prepared from the following raw materials in percentage by mass:
dissolving aminoethyl aminopropyl polydimethylsiloxane into cyclohexanone, adding a mixed filler consisting of aluminum powder, ferrophosphorus powder, mica powder and talcum powder into a system, dispersing and mixing uniformly, and grinding the mixture to be less than 10 microns by using a grinder. And (3) uniformly mixing the mixture obtained by grinding with a styrene maleic anhydride copolymer, coating the mixture on a metal substrate, and heating the metal substrate at the temperature of 160 ℃ for 30 minutes to obtain the organosilicon coating with a rigid molecular structure. The long-term service temperature of the coating is more than 450 ℃, the salt spray resistance of the coating after high temperature (according to GB/T1771-2007) is 12 days, the adhesion (according to GB/1720-89) is 0 grade, the curing temperature is not more than 160 ℃, the curing time is not more than 1H, the hardness (according to GB/T6739-2006) is 6H, and the flexibility (according to GB/T1731 and 1993) of the coating is 4 mm.
Example 6:
the organic silicon coating with the rigid molecular structure is prepared from the following raw materials in percentage by mass:
dissolving aminoethyl aminopropyl polydimethylsiloxane into cyclohexanone, adding a mixed filler consisting of aluminum powder, ferrophosphorus powder, mica powder and talcum powder into a system, dispersing and mixing uniformly, and grinding the mixture to be less than 10 microns by using a grinder. And (3) uniformly mixing the mixture obtained by grinding with a styrene maleic anhydride copolymer, coating the mixture on a metal substrate, and heating the metal substrate at the temperature of 160 ℃ for 30 minutes to obtain the organosilicon coating with a rigid molecular structure. The long-term service temperature of the coating is more than 460 ℃, the salt spray resistance of the coating after high temperature (according to GB/T1771-2007) is 12 days, the adhesion (according to GB/1720-89) is 0 grade, the curing temperature is not more than 160 ℃, the curing time is not more than 1H, the hardness (according to GB/T6739-2006) is 6H, and the flexibility (according to GB/T1731 and 1993) of the coating is 4 mm.
Claims (10)
1. The organic silicon coating with the rigid molecular structure is characterized by comprising aminoethyl aminopropyl polydimethylsiloxane, styrene maleic anhydride copolymer, mixed filler and cyclohexanone, wherein the mass percent of each component is as follows:
35-45% of aminoethylaminopropylpolydimethylsiloxane;
5-10% of styrene maleic anhydride copolymer;
20-30% of mixed filler;
25-30% of cyclohexanone
The preparation method comprises the following steps: dissolving aminoethyl aminopropyl polydimethylsiloxane into cyclohexanone, adding mixed filler into a system, dispersing and mixing uniformly, and grinding the mixture to be less than 10 microns by using a grinder; the mixture obtained by grinding is evenly mixed with styrene maleic anhydride copolymer and then coated on a metal substrate, and the metal substrate is heated for 30 minutes at the temperature of 80 ℃ and then heated for 30 minutes at the temperature of 160 ℃.
2. The organosilicon coating with a rigid molecular structure according to claim 1, wherein the mass percentage of each component is:
43% of aminoethylaminopropyl polydimethylsiloxane;
9% of styrene maleic anhydride copolymer;
22% of mixed filler;
and 26% of cyclohexanone.
3. The silicone coating material with a rigid molecular structure according to claim 1 or 2, wherein the styrene maleic anhydride copolymer is in a powder form.
4. The silicone coating material with a rigid molecular structure according to claim 1 or 2, wherein the acid value of the styrene maleic anhydride copolymer is 355.
5. The silicone coating material with a rigid molecular structure according to claim 4, wherein the number average molecular weight of the styrene maleic anhydride copolymer is 3000, and the weight average molecular weight is 750.
6. The silicone coating material with a rigid molecular structure according to claim 1 or 2, wherein the mixed filler is composed of aluminum powder, ferrophosphorus powder, mica powder and talc powder.
7. The organosilicon coating with a rigid molecular structure according to claim 6, wherein the aluminum powder, the ferrophosphorus powder, the mica powder and the talcum powder are mixed according to a mass ratio of 1:2:6: 5.
8. A preparation method of an organosilicon coating with a rigid molecular structure is characterized in that aminoethyl aminopropyl polydimethylsiloxane is dissolved in cyclohexanone, then mixed filler is added into a system, and the mixture is ground to be below 10 microns by a grinder after being dispersed and mixed uniformly; uniformly mixing the mixture obtained by grinding with a styrene maleic anhydride copolymer, coating the mixture on a metal base material, heating the mixture at the temperature of 80 ℃ for 30 minutes, and heating the mixture at the temperature of 160 ℃ for 30 minutes, wherein the mass percentage of each component is as follows:
35-45% of aminoethylaminopropylpolydimethylsiloxane;
5-10% of styrene maleic anhydride copolymer;
20-30% of mixed filler;
25-30% of cyclohexanone.
9. The method for preparing the organosilicon coating with the rigid molecular structure according to claim 8, wherein the mixed filler is composed of aluminum powder, ferrophosphorus powder, mica powder and talcum powder according to a mass ratio of 1:2:6: 5.
10. The method of claim 8, wherein the styrene maleic anhydride copolymer is in the form of powder, and has an acid value of 355, a number average molecular weight of 3000, and a weight average molecular weight of 750.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432752A (en) * | 2011-08-18 | 2012-05-02 | 江苏科技大学 | Styrene-maleic anhydride copolymer imidization material and preparation method thereof |
| CN103025799A (en) * | 2010-07-27 | 2013-04-03 | 瓦克化学股份公司 | Process for producing siloxane copolymers with urethane-sulphonamido linking groups |
| WO2016064481A1 (en) * | 2014-10-22 | 2016-04-28 | The Government Of The United States Of America, As Represented By The Secretary Of The Navy | Two-component siloxane-based coatings containing polymers with urea linkages and terminal alkoxysilanes |
| CN107141911A (en) * | 2017-07-07 | 2017-09-08 | 佛山领新信息科技有限公司 | Exterior coating that a kind of drying time is short and adhesive property is strong and preparation method thereof |
| CN107556750A (en) * | 2017-07-24 | 2018-01-09 | 四川大学 | High temperature resistant polyetherimide amido composite foam material and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150240125A1 (en) * | 2013-08-09 | 2015-08-27 | Teknologisk Institut | Repellent Coating Composition and Coating, Method for Making and Uses Thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103025799A (en) * | 2010-07-27 | 2013-04-03 | 瓦克化学股份公司 | Process for producing siloxane copolymers with urethane-sulphonamido linking groups |
| CN102432752A (en) * | 2011-08-18 | 2012-05-02 | 江苏科技大学 | Styrene-maleic anhydride copolymer imidization material and preparation method thereof |
| WO2016064481A1 (en) * | 2014-10-22 | 2016-04-28 | The Government Of The United States Of America, As Represented By The Secretary Of The Navy | Two-component siloxane-based coatings containing polymers with urea linkages and terminal alkoxysilanes |
| CN107141911A (en) * | 2017-07-07 | 2017-09-08 | 佛山领新信息科技有限公司 | Exterior coating that a kind of drying time is short and adhesive property is strong and preparation method thereof |
| CN107556750A (en) * | 2017-07-24 | 2018-01-09 | 四川大学 | High temperature resistant polyetherimide amido composite foam material and preparation method thereof |
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Effective date of registration: 20220613 Address after: 511500 Xingyuan Road, Qingyuan National Industrial Park, Lianzhou City, Qingyuan City, Guangdong Province (lot 0638100015) Patentee after: QINGYUAN WEICHANGDA CHEMICAL CO.,LTD. Address before: 201800 358 Kefu Road, Jiading District, Shanghai_ Room j2644, Zone E, floor 1, building 4, No. 368 Patentee before: Shanghai Yiyou Information Technology Co.,Ltd. Effective date of registration: 20220613 Address after: 201800 358 Kefu Road, Jiading District, Shanghai_ Room j2644, Zone E, floor 1, building 4, No. 368 Patentee after: Shanghai Yiyou Information Technology Co.,Ltd. Address before: 212003, No. 2, Mengxi Road, Zhenjiang, Jiangsu Patentee before: JIANGSU University OF SCIENCE AND TECHNOLOGY |