CN101081962A - Epoxy resin modified organosilicon fire-resistant anticorrosion paint - Google Patents
Epoxy resin modified organosilicon fire-resistant anticorrosion paint Download PDFInfo
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Abstract
The present invention relates to one kind of epoxy resin modified heat resistant anticorrosive organosilicon paint, which consists of two components, including one component A comprising epoxy resin modified organosilicon 30-40 wt%, pigment, stuffing and assistant 20-35 wt%, and solvent 25-50 wt%; and one component B of liquid polyamide resin in the amount of 7-20 wt% of the component A. Of the paint, the epoxy resin modified organosilicon is prepared with organosilicon pre-polymer and through modification with epoxy resin. The heating cured coating formed with the paint has excellent performances, including high structural stability, high heat resistance, high water tolerance, high organic solvent tolerance, high acid and alkali resistance, high weather resistance, etc. and is suitable for industrial application.
Description
Technical field
Invention relates to a kind of epoxy resin modified organosilicon coating that is used for high-temperature resistant anti-corrosive.
Background technology
Traditional organic anti-corrosive coating, the very fast fracture of its molecular chain is at high temperature decomposed, thereby causes the inefficacy of filming.And many coating that are applied to high-temperature resistant anti-corrosive, as organic fluorine, polyphenylene sulfide, polyarylsulphone, polyimide etc., perhaps cost is too high, and perhaps difficulty is solidified in construction, is difficult to obtain to use widely.Other inorganic high-temperature resistant material also exists similar problem.Organosilicon material is applicable to the multiple application of indoor and outdoors because stablizing of siloxane bond bond energy has good weathering resistance, thermotolerance, gloss retention, antiacid rain etc.Again because of containing snappiness and the easy machining characteristics that organic group has macromolecular material in the side chain.Both are in conjunction with making it have concurrently organic and two-fold advantage inorganic materials, as the performances such as protection against the tide, hydrophobic, electric insulation, high-low temperature resistant, chemically stable and physiology inertia of excellence.But pure organosilicon coating sticking power and organic solvent resistance are poor; And solidification value height, set time long (as needing to solidify about 1h at 225 ℃), be not easy to large-area construction, so directly the filmogen as coating is restricted.For giving full play to the advantage of silicone resin, overcome its shortcoming simultaneously, available organic resin carries out modification to it.
Modified organic silicone resin has following several approach: 1. physics method, also be cold spelling, promptly mix and form with organic resin and the cold assembly of silicone resin (phenyl content is higher usually) good with its intermiscibility, this method technology is simple, but modified effect is good not as the chemical process modification;
2. transition method promptly adds organosilicon superpolymer and the 3rd component high-molecular copolymer with transition phase function, as silane coupling agent etc., in mixing process, has the effect of physics and chemical two aspects to take place simultaneously, and effect is better than the physics method.
3. chemical method, promptly with the active group (hydroxyl) of organic resin under appropriate reaction conditions, with the hydroxyl in the silicone intermediate oligopolymer, alkoxyl group or unsaturated alkyl carry out polycondensation or polyreaction, make modified organic silicon.
This patent adopts Resins, epoxy and silicone resin to carry out chemical modification, is aided with high temperature resistant color stuffing and auxiliary agent, and coating structure is stable, and is high temperature resistant, water-fast, anti-solvent, acid and alkali-resistance, performances such as weathering resistance are all very excellent, are applicable to industrial application, are with a wide range of applications.
At present, organosilicon and various modified paint thereof have been widely used in the high-temperature resistant anti-corrosive field.But mostly existing patent is pure organosilicon, or the modified organic silicon that makes with physics method and transition method, the fire-resistant anticorrosion paint of purposes such as the report of the epoxy resin modified organosilicon cold coating of rare chemical method also seldom has to relate to be applied to interchanger, and high-temperature pipe is anticorrosion.U.S. Pat 4121000 has been described a kind of by polyorganosiloxane resin type prepolymer, fluorocarbon polymer, and Resins, epoxy, and organosilicon fluid, the coating compound that a kind of inorganic hardener is formed, filming behind this paint solidification has thermostability, high gloss, hardness, abrasion resistance, to not priming, untreated metal material surface has excellent sticking power, is applicable to cooker.
U.S. Pat 5317046 in 1994, relate to a kind of aqueous polyamide-epoxy-organic silicon ternary compound coating, this coating has good snappiness and hardness, and good chemical proofing, low VOC content, but air curing, but be not suitable for protection against corrosion, do not see the report that related application is arranged yet.
CN1560156A has described a kind of pure organosilicon coating, is applied to high temperature resistantly, and its used silicone resin is a phenyl chlorosilane, the hydrolysate of methyl chlorosilane, added certain fluorine silicoorganic compound, had normal temperature quick-drying, the advantage that paint film is tough and tensile and cheap.But do not see yet the report of this application of paints in corrosion-resistant field arranged.
Summary of the invention
The purpose of this invention is to provide a kind of high temperature resistant, and the protective coating of the common medium of chemical industry such as ability hot water, oil, acid, alkali, this coating has the mechanical property excellence, low cost and other advantages.
A kind of epoxy resin modified organosilicon fire-resistant anticorrosion paint of the present invention is made of component A component A, B component: epoxy resin modified organosilicon, and the mass percent of its component is as follows:
(1) matrix resin: epoxy resin modified organosilicon 30%～40%;
(2) color stuffing and auxiliary agent: 20%～35%;
(3) solvent: 25%～50%;
B component: polymeric amide liquid resin, its consumption are 7%～20% of component A;
Coating of the present invention, epoxy resin modified organosilicon solution is made through epoxy resin modification by the silicone intermediate prepolymer, and its working method is as follows:
(1) silicone intermediate prepolymer preparation: with the monomethyl triethoxyl silane, dimethyl diethoxy grade silane, one phenyl triethoxysilane monomer and xylene solvent add in the reactor, the monomethyl triethoxyl silane, dimethyldiethoxysilane, the monomeric mass ratio of one phenyl triethoxysilane is 6: 5: 8, reactor is heated to 60～70 ℃, add hydrochloric acid again as catalyzer, 70%～100% of slow adding complete hydrolysis amount water under agitation condition, reacted 3～5 hours, add the alkali neutralization reaction product then, after filtration, by product is removed in distillation and partial solvent makes the silicone intermediate pre-polymer solution;
(2) preparation of epoxy resin modified organosilicon solution: silicone intermediate pre-polymer solution and Resins, epoxy mix by 1: 0.42 by mass ratio 1: 1.5, under 130～170 ℃, add naphthenate as modification promotor, reacted 3～5 hours, obtain epoxy resin modified organosilicon; Add the inert solvent dilution, obtain the epoxy resin modified organosilicon solution of solid content 50%.
The silicone intermediate prepolymer that the present invention adopts is a solvent with dimethylbenzene, and solid content 60% is the 30-50 centipoise 25 degrees centigrade of following viscosity, and proportion is 1.03-1.2, and specific refractory power is 1.45-1.57.
The Resins, epoxy that the present invention adopts is that oxirane value is 0.18-0.22, and softening temperature 64-78 ℃ bisphenol A epoxide resin can be selected the Resins, epoxy of the E-20 or the close trade mark for use.
In the coating of the present invention, B component polymeric amide liquid resin is a solidifying agent, and 180～220,40 ℃ of following viscosity of its amine value are 1500～25000 centipoises, and proportion is about 0.99, reactive hydrogen equivalent about 210.
The color stuffing that adopts in the coating of the present invention is talcum powder, mica powder, carbon black, graphite, molybdenumdisulphide, zinc phosphate or aluminium powder.Auxiliary agent is flow agent and coupling agent.
The invention provides a kind of epoxy resin modified organosilicon fire-resistant anticorrosion paint, the resin matrix of this coating is made by silicone intermediate and the Resins, epoxy catalyzed reaction that the methylphenyl siloxane hydrolysis obtains.This coating comprises resin matrix, color stuffing and auxiliary agent and inert solvent thinner, uses low-molecular-weight polyamide resin as solidifying agent during use.
The silicone intermediate prepolymer that present method makes can be stabilized in room temperature and deposit above 3 months.
This coating can adopt dimethyl polysiloxane as flow agent, and the consumption of dimethyl polysiloxane depends on the gross weight of matrix resin, and its consumption is 0.2%～10% of a matrix resin consumption, and optimum consumption is 0.5～3%.
This coating can adopt KH-560 as coupling agent, and its consumption is 0.5%～1.0% of a matrix resin consumption, and its effect can improve the sticking power of coating to ground, and promotes the dispersion of color stuffing in resin matrix to reduce system viscosity.
This coating can adopt the solidifying agent of a kind of low-molecular-weight polyamide resin as modified organosilicon paint, and this solidifying agent should add in the coating before paint spraying, and thorough mixing is even.
Concrete coating process is: ground must can adopt means such as polishing, chemical rust removing through certain pre-treatment, and is then better if any operations such as bonderizing.Application can an application, and also application several times is to obtain thicker paint film.Film thickness should be less than 50 μ m, usually should be between 50～150 μ m.The curing process of filming is: 150～200 ℃, 30min promptly obtained solidified and filmed set time.This good heat resistance of filming can stand the high temperature below 300 ℃ for a long time, excellent corrosion resistance, the long-term non-corroding of boiling water boiling, the high temperature corrosion of energy acid-and base-resisting and oils.The paint film satisfactory mechanical property can satisfy various uses.Coating of the present invention can be applicable to the heat-resistant anticorrosive field, especially the corrosion prevention of environment such as hot water, oil, acid, alkali.
Embodiment
Embodiment 1
(1) preparation method of silicone intermediate prepolymer: with mass ratio is that 6: 5: 8 monomethyl triethoxyl silane, dimethyl diethoxy grade silane, a phenyl triethoxysilane monomer mixes, the dimethylbenzene that adds equal in quality is as solvent, the HCl of use 0.1% is as catalyzer, 70% of adding complete hydrolysis amount water under 70 ℃ of conditions, stir, reacted 5 hours, neutralization reaction product then, filter, by product and partial solvent are removed in distillation, are at room temperature deposited stable intermediate prepolymer.
(2) use the intermediate prepolymer that makes in above-mentioned (1) and solid content 50%, oxirane value is 0.18-0.22, softening temperature 64-78 ℃ Resins, epoxy (E-20 Resins, epoxy) reaction, mass ratio 1: 1, temperature: 140 ℃, add the curing catalyst of the zinc naphthenate of 0.5% zinc value 8%-9%, survey the gelation time decision termination time as modified resin.Final product is the epoxy resin modified organosilicon resin, adds an amount of dimethylbenzene cut back, and making solid content is 50%.
(3) modified organic silicone resin and the color stuffing that obtains with above-mentioned (2) mixes by following prescription: (mass ratio)
Modified organic silicone resin solution: 60g
Talcum powder: 10g
Kaolin: 10g
Mica powder: 5g
Molybdenumdisulphide: 5g
Graphite Powder 99: 5g
Carbon black: 5g
Flow agent 801A:1g
Coupling agent KH-560:0.5g;
The polymeric amide liquid resin (650# or analogous products) that adds 10g before use adopts high speed dispersor fully to disperse.
Adopt above-mentioned coating that model is carried out three applications, obtain film thickness: 120 μ m.Solidify through 150 ℃ of 30min, obtain smooth and hard filming, the physical and mechanical properties that test is filmed is as follows:
| Project | Index | Experimental technique |
| 1. paint film color and outward appearance | Black, smooth smooth | Range estimation |
| 2. viscosity (being coated with 4 glasss) | 40s | GB1723 |
| 3. sticking power | 1 grade | GB1720 |
| 4. thermotolerance (300 ℃ of 100h) | Complete | GB1735 |
| 5. anti-boiling water (48h) | Complete, there is not serious corrosion | GB1733-93 |
| 6.10％NaOH(300h) | Complete, there is not serious corrosion | GB1763-93 |
| 7. anti-solvent | Toluene, 200h passes through |
Embodiment 2
(1) preparation method of silicone intermediate prepolymer is with embodiment 1.
(2) synthetic method of modified organic silicone resin changes modification promotor into 0.5% cobalt naphthenate with embodiment 1, and other conditions are constant
(3) adopt following prescription to mix:
Modified organic silicone resin solution: 60g
Talcum powder: 5g
Kaolin: 10g
Mica powder: 5g
Zinc phosphate: 10g
Titanium dioxide: 10g
Flow agent 801A:1g
Coupling agent KH-560:0.5g;
The polymeric amide liquid resin (650#) that adds 10g before use adopts high speed dispersor fully to disperse.
Adopt above-mentioned coating that model is carried out three applications, obtain film thickness: 120 μ m.Solidify through 150 ℃ of 30min, obtain smooth and hard filming, the physical and mechanical properties that test is filmed is as follows:
| Project | Index | Experimental technique |
| 1. paint film color and outward appearance | White, smooth smooth | Range estimation |
| 2. viscosity (being coated with 4 glasss) | 45s | GB1723 |
| 3. sticking power | 1 grade | GB1720 |
| 4. thermotolerance (300 ℃ of 100h) | Complete | GB1735 |
| 5. anti-boiling water (48h) | Complete, there is not serious corrosion | GB1733-93 |
| 6.10％NaOH(300h) | Complete, there is not serious corrosion | GB1763-93 |
| 7. anti-solvent | Toluene, 200h passes through |
Embodiment 3
(1) preparation method of silicone intermediate prepolymer is with embodiment 1.
(2) synthetic method of modified organic silicone resin is with embodiment 1,
(3) adopt following prescription to mix:
Modified organic silicone resin solution: 50g
Kaolin: 10g
Mica powder: 10g
Molybdenumdisulphide: 10g
Zinc phosphate: 18g
Flow agent 801A:1g
Coupling agent KH-560:0.5g;
The polymeric amide liquid resin (650# or analogous products) that adds 10g before use adopts high speed dispersor fully to disperse.
Adopt above-mentioned coating that model is carried out three applications, obtain film thickness: 120 μ m.Solidify through 150 ℃ of 30min, obtain smooth and hard filming, the physical and mechanical properties that test is filmed is as follows:
| Project | Index | Experimental technique |
| 1. paint film color and outward appearance | White, smooth smooth | Range estimation |
| 2. viscosity (being coated with 4 glasss) | 40s | GB1723 |
| 3. sticking power | 1 grade | GB1720 |
| 4. thermotolerance (300 ℃ of 2h) | Complete, little yellowing | GB1735 |
| 5. anti-boiling water (24h) | Complete, there is not serious corrosion | GB1733-93 |
| 6.10％NaOH(300h) | Complete, there is not serious corrosion | GB1763-93 |
| 7. anti-solvent | Toluene, 200h passes through |
Embodiment 4
(1) preparation method of silicone intermediate prepolymer is with embodiment 1.
(2) synthetic method of modified organic silicone resin is with embodiment 1,
(3) adopt following prescription:
Modified organic silicone resin solution: 50g
Talcum powder: 10g
Lime carbonate: 10g
Kaolin: 10g
Mica powder: 10g
Aluminium powder: 5g
Flow agent 801A:1g
Coupling agent KH-560:0.5g;
The polymeric amide liquid resin (650#) that adds 10g before use adopts high speed dispersor fully to disperse.
Adopt above-mentioned coating that model is carried out three applications, obtain film thickness: 120 μ m.Solidify through 150 ℃ of 30min, obtain smooth and hard filming, the physical and mechanical properties that test is filmed is as follows:
| Project | Index | Experimental technique |
| 1. paint film color and outward appearance | The silvery white metallic color, smooth | Range estimation |
| 2. viscosity (being coated with 4 glasss) | 75s | GB1723 |
| 3. sticking power | 1 grade | GB1720 |
| 4. thermotolerance (300 ℃ of 100h) | Little yellowing | GB1735 |
| 5. anti-boiling water (24h) | Bubble a little | GB1733-93 |
| 6.100％NaOH(300h) | Complete, there is not serious corrosion | GB1763-93 |
| 7. anti-solvent | The acetone wiping, duskiness |
Claims (6)
1. an epoxy resin modified organosilicon fire-resistant anticorrosion paint is made of component A, B component, it is characterized in that:
Component A: epoxy resin modified organosilicon, the mass percent of its component is as follows:
(1) matrix resin: epoxy resin modified organosilicon 30%～40%;
(2) color stuffing and auxiliary agent: 20%～35%;
(3) solvent: 25%～50%;
B component: polymeric amide liquid resin, its consumption are 7%～20% of component A;
2. coating according to claim 1 is characterized in that: epoxy resin modified organosilicon solution is made through epoxy resin modification by the silicone intermediate prepolymer, and its working method is as follows:
(1) silicone intermediate prepolymer preparation: with the monomethyl triethoxyl silane, dimethyl diethoxy grade silane, one phenyl triethoxysilane monomer and xylene solvent add in the reactor, the monomethyl triethoxyl silane, dimethyldiethoxysilane, the monomeric mass ratio of one phenyl triethoxysilane is 6: 5: 8, reactor is heated to 60～70 ℃, add hydrochloric acid again as catalyzer, 70%～100% of slow adding complete hydrolysis amount water under agitation condition, reacted 3～5 hours, add the alkali neutralization reaction product then, after filtration, by product is removed in distillation and partial solvent makes the silicone intermediate pre-polymer solution;
(2) preparation of epoxy resin modified organosilicon solution: silicone intermediate pre-polymer solution and Resins, epoxy mix by 1: 0.42 by mass ratio 1: 1.5, under 130～170 ℃, add naphthenate as modification promotor, reacted 3～5 hours, obtain epoxy resin modified organosilicon; Add the inert solvent dilution, obtain the epoxy resin modified organosilicon solution of solid content 50%.
3. silicone intermediate prepolymer according to claim 2 is characterized in that: be solvent with dimethylbenzene, solid content 60% is the 30-50 centipoise 25 degrees centigrade of following viscosity, and proportion is 1.03-1.2, and specific refractory power is 1.45-1.57.
4. Resins, epoxy according to claim 2 is characterized in that: this Resins, epoxy is that oxirane value is 0.18-0.22, softening temperature 64-78 ℃ bisphenol A epoxide resin.
5. coating according to claim 1 is characterized in that: B component polymeric amide liquid resin is a solidifying agent, and 180～220,40 ℃ of following viscosity of its amine value are 1500～25000 centipoises, and proportion is about 0.99, reactive hydrogen equivalent 210.
6. coating according to claim 1 is characterized in that: in color stuffing and the auxiliary agent: color stuffing is talcum powder, mica powder, carbon black, graphite, molybdenumdisulphide, zinc phosphate or aluminium powder; Auxiliary agent is flow agent and coupling agent.
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