CN102585696A - Methyl phenyl silicone resin base high-temperature-resistant coating and preparation method thereof - Google Patents
Methyl phenyl silicone resin base high-temperature-resistant coating and preparation method thereof Download PDFInfo
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Abstract
The invention relates to methyl phenyl silicone resin base high-temperature-resistant coating and a preparation method thereof, which belong to the technical field of organic coating preparation. Methyl phenyl silicone resin serves as a base stock. The resin utilizes methyl trichlorosilane, dimethyldichlorosilance and methylphenyldichloros as hydrolysis raw materials and is prepared by processes of hydrolysis, polycondensation and the like. The preparation process is simple, the resin yield is high, and the pure resin itself has good high temperature resistance and low temperature resistance. The coating utilizes titanium dioxide as pigment, mica powder, talcum powder, low melting-point glass powder and hollow glass microspheres as fillers, organobentonite and KH-550 as auxiliaries and dimethylbenzene as solvent. Organosilicone high-temperature-resistant coating prepared by the preparation method is coated on the surface of a base material, is fast in air drying speed at normal temperature, tough in coating film and high in mechanical strength, can resist to the high temperature of 1000 DEG C for a long time, and has long salt fog resistance time. In addition, the impact strength of the high-temperature-resistant coating reaches above 50kg.cm.
Description
Technical field
The present invention relates to a kind of high temperature organosilicon paint and preparation method thereof, belong to the organic coating preparing technical field.Refering in particular to the methyl phenyl silicone resin is base-material, adds various face, filler, the method for synthetic long-term anti-1000 ℃ of high temperature, corrosion resistant organosilicon coating in solvent.
Technical background
Organosilicon polymer be a veriety numerous, have the unique physical and chemical performance and novel Chemicals of applied range.Since the forties in 20th century, Industrial products came out, organosilicon polymer obtained to develop rapidly.At present; With all kinds of silane monomers, siloxanes midbody and the silicone oil that is made by them, Zylox, silicone resin is the various products of base-material preparation; Fields such as electron and electrician, automobile, weaving, building, makeup, medical treatment, chemical industry, aerospace have been widely used in; Especially at high-technology field very important effect is arranged, be described as " catalyzer of hi-tech development ".High temperature organosilicon paint is one of organosilyl staple product, has fabulous researchdevelopment space.
High-temperature resistant coating refers generally to temperature in paint film nondiscoloration more than 200 ℃, do not come off, and still can keep the coating of good physical and mechanical properties.Positions such as some high temperature steam pipelines, High Temperature Furnaces Heating Apparatus, petroleum cracking equipment, mover and vapor pipe are in the hot environment for a long time; High temperature corrosion is serious; Increased the ME expense, had very big safety in production hidden danger, therefore adopting the high-temperaure coating protection is a kind of efficient ways.Industry in modern times, military affairs, aerospace field have wide application prospect.It is reported that the high-temperature resistant coating of having developed at present is 1400 ℃ of high temperature of ability at least abroad.And China's research in this respect falls behind, and the report of 700 ℃ of high-temperature coatings of ability is few, and the main at present import external product that relies on consumes a large amount of foreign exchanges every year.
Patent CN 101255312A discloses ultra heat-resistant coating of a kind of solvent-type organosilicon and working method thereof, 500 ℃ of high temperature of the highest ability of organosilicon coating that this method is produced.Patent CN 10105496A discloses a kind of working method of organosilicon heat-resistant coating, heating 10 min under 800 ℃ of temperature, and coating is excellent, but the said complicated process of preparation of this method.High temperature organosilicon paint of the present invention can be heat-resisting for a long time under 1000 ℃, and preparation technology is simple, is present better heat-resisting protective system.Be characterized in: 1. the normal temperature self-drying of filming is fast, paint film is tough and tensile, the alternating hot and cold performance is good, bonding force is strong; 2. filming can be heat-resisting for a long time under 1000 ℃, and it is good at substrate surface sticking power to film, and resistance to impact shock reaches more than the 50 ㎏ ㎝.But application is used for heat-resisting boiler, high temperature steam pipeline, automobile and thrust chamber etc., has good anti-corrosion and salt fog resistance; 3. silicone resin is the self-control methyl phenyl silicone resin, and preparation technology is simple, and production cost is low.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of methyl phenyl silicone resin based high-temp-resistant coating.Its characteristics are that the methyl phenyl silicone resin base-material that is adopted is homemade silicone resin, and preparation technology is simple, and production cost is low.With this resin is that the base-material prepared coating can be heat-resisting for a long time under 1000 ℃, and filming can be at room temperature dry voluntarily, and paint film is tough and tensile, physical strength is high, has good anti-corrosion and salt fog resistance.
The technical scheme that the present invention adopts is:
A kind of methyl phenyl silicone resin based high-temp-resistant coating is prepared from following weight percent proportion raw material:
Methyl phenyl silicone resin: 20 ~ 40 parts,
High-temperature resisting pigment pigment: 5 ~ 30 parts,
Filler: 35 ~ 50 parts,
Auxiliary agent: 1 ~ 5 part,
Solvent is an amount of: 5 ~ 16 parts.
Preferably be prepared from following weight percent proportion raw material:
Methyl phenyl silicone resin: 25 ~ 35 parts,
High-temperature resisting pigment: 10 ~ 25 parts,
Filler: 40 ~ 45 parts,
Auxiliary agent: 3 parts,
Solvent is an amount of: 5 ~ 16 parts.
Wherein said high-temperature resisting pigment is a white titanium pigment;
Wherein said filler is one or more of mica powder, talcum powder, glass powder with low melting point or hollow glass microballoon;
Wherein said auxiliary agent be organobentonite or KH-550 one or both;
Wherein said solvent is YLENE or toluene; Or the mixed solvent of toluene and YLENE.
The preparation method of above-mentioned a kind of methyl phenyl silicone resin based high-temp-resistant coating; Carry out according to following step: with the methyl phenyl silicone resin is base-material, under the normal temperature, after resin is uniformly dispersed in solvent; Add high-temperature resisting pigment and filler; Grind 2 h at skin grinder, add auxiliary agent etc. again, filter the coating that gets product.
The invention has the advantages that:
1. the prepared high temperature organosilicon paint of the present invention is coated on substrate surface, and normal temperature self-drying speed is fast, about 30 ~ 40 min; Film tough and tensile, physical strength is high.
Described base material is stainless steel plate or tinplate tin sheet.
2. the prepared high temperature organosilicon paint of the present invention can long-term anti-1000 ℃ of high temperature, the complete no change of filming, and alternating hot and cold is functional; It is good at substrate surface sticking power to film, and resistance to impact shock reaches more than the 50 ㎏ ㎝, and salt fog resistance reaches as high as 18 d.
3. the resin binder that the present invention adopted is the self-control methyl phenyl silicone resin, and its preparation technology is simple, and virgin resin self resistance toheat resistance toheat is good.
4. the face that the present invention adopted, filler and auxiliary agent be simple and easy to and cheap, the coating material production cost is low, has good economy, environment and social benefit.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail, but embodiment of the present invention is not limited thereto.
The methyl phenyl silicone resin base-material that the present invention adopted is the self-control resin; This resin thinks that METHYL TRICHLORO SILANE, dimethyldichlorosilane(DMCS) and dichloromethyl phenylsilane are raw material, obtain the methyl phenyl silicone resin that solid content is 50 % ~ 60 % through technologies such as hydrolysis, polycondensations.Concrete preparation method is following: (addition is 60.4 in 1000 mL four-hole boiling flasks, to add a certain amount of METHYL TRICHLORO SILANE and dimethyldichlorosilane(DMCS)
WtThe % METHYL TRICHLORO SILANE, if no special instructions, below the addition of each material be the mass percent with METHYL TRICHLORO SILANE), dichloromethyl phenylsilane (38.3
Wt%), YLENE (299.8
Wt%) and acetone (120.4
Wt%), mix, ice-water bath keeps down fully stirring, to wherein dripping water (486.5
Wt%) and acetone (243.2
WtMixture %) keeps 6 ~ 8 h to dropwise.Fully stir and continue reaction 8 h.Get the upper strata oil-reservoir water after reaction finishes and be washed till neutrality, obtain the white opacity prepolymer.Add TMAH (0.8 in the prepolymer
Wt%) condensation catalyst reacts 6 h in 130 ℃ of refluxed.Reaction finishes the decompression under 100 ℃ of back solution and takes off partial solvent, and the control solid content is that 50 % ~ 60 % are terminal point.The gained methyl phenyl silicone resin is a transparent flow liquid.
Embodiment 1
Stirring sand milling dispersion machine 35 kilograms of methyl phenyl silicone resins of adding and 16 kilograms of YLENE, agitating resin is uniformly dispersed in solvent.To wherein adding 25 kilograms of white titanium pigments, 10 kilograms of talcum powder, 12 kilograms of mica powders and 1 kilogram of organobentonite, dispersed with stirring 4 h respectively.Add 1 kilogram of KH-550 sand milling 2 h again, filter the coating that gets product.
With prepared coating be coated on oil removing, rust cleaning and the stainless steel plate handled with YLENE in advance on, do solid work brushing second road, back, coating thickness is controlled at about 50 μ m.Treat to carry out resistance toheat, resistance to impact shock, sticking power test and erosion resistance test behind the curing of coating, the result sees table 1.
Embodiment 2
In stirring the sand milling dispersion machine, add 35 kilograms of methyl phenyl silicone resins and 16 kilograms of YLENE, agitating resin is uniformly dispersed in solvent.To wherein adding 12 kilograms of white titanium pigments, 10 kilograms of talcum powder, 25 kilograms of mica powders and 1 kilogram of organobentonite, dispersed with stirring 4 h respectively.Add 1 kilogram of KH-550 sand milling 2 h again, filter the coating that gets product.
With prepared coating be coated on oil removing, rust cleaning and the stainless steel plate handled with YLENE in advance on, do solid work brushing second road, back, coating thickness is controlled at about 50 μ m.Treat to carry out resistance toheat, resistance to impact shock, sticking power test and erosion resistance test behind the curing of coating, the result sees table 1.
Embodiment 3
Stirring sand milling dispersion machine 35 kilograms of methyl phenyl silicone resins of adding and 16 kilograms of YLENE, agitating resin is uniformly dispersed in solvent.To wherein adding 25 kilograms of glass powder with low melting point, 10 kilograms of white titanium pigments, 10 kilograms of talcum powder, 12 kilograms of mica powders and 1 kilogram of organobentonite, dispersed with stirring 4 h respectively.Add 1 kilogram of KH-550 sand milling 2 h again, filter the coating that gets product.
With prepared coating be coated on oil removing, rust cleaning and the stainless steel plate handled with YLENE in advance on, do solid work brushing second road, back, coating thickness is controlled at about 50 μ m.Treat to carry out resistance toheat, resistance to impact shock, sticking power test and erosion resistance test behind the curing of coating, the result sees table 1.
Embodiment 4
In stirring the sand milling dispersion machine, add 35 kilograms of methyl phenyl silicone resins and 5 kilograms of YLENE, agitating resin is uniformly dispersed in solvent.To wherein adding 35 kilograms of glass powder with low melting point, 10 kilograms of talcum powder, 12 kilograms of mica powders and 2 kilograms of organobentonites, dispersed with stirring 4 h respectively.Add 1 kilogram of KH-550 sand milling 2 h again, filter the coating that gets product.
With prepared coating be coated on oil removing, rust cleaning and the stainless steel plate handled with YLENE in advance on, do solid work brushing second road, back, coating thickness is controlled at about 50 μ m.Treat to carry out resistance toheat, resistance to impact shock, sticking power test and erosion resistance test behind the curing of coating, the result sees table 1.
Embodiment 5
In stirring the sand milling dispersion machine, add 30 kilograms of methyl phenyl silicone resins and 10 kilograms of YLENE, agitating resin is uniformly dispersed in solvent.To wherein adding 25 kilograms of glass powder with low melting point, 10 kilograms of white titanium pigments, 10 kilograms of talcum powder, 12 kilograms of mica powders and 2 kilograms of organobentonites, dispersed with stirring 4h respectively.Add 1 kilogram of KH-550 sand milling 2h again, filter the coating that gets product.
With prepared coating be coated on oil removing, rust cleaning and the stainless steel plate handled with YLENE in advance on, do solid work brushing second road, back, coating thickness is controlled at about 50 μ m.Treat to carry out resistance toheat, resistance to impact shock, sticking power test and erosion resistance test behind the curing of coating, the result sees table 1.
Embodiment 6
In stirring the sand milling dispersion machine, add 25 kilograms of methyl phenyl silicone resins and 10 kilograms of YLENE, agitating resin is uniformly dispersed in solvent.To wherein adding 30 kilograms of glass powder with low melting point, 10 kilograms of white titanium pigments, 10 kilograms of talcum powder, 12 kilograms of mica powders and 2 kilograms of organobentonites, dispersed with stirring 4 h respectively.Add 1 kilogram of KH-550 sand milling 2 h again, filter the coating that gets product.
With prepared coating be coated on oil removing, rust cleaning and the stainless steel plate handled with YLENE in advance on, do solid work brushing second road, back, coating thickness is controlled at about 50 μ m.Treat to carry out resistance toheat, resistance to impact shock, sticking power test and erosion resistance test behind the curing of coating, the result sees table 1.
Embodiment 7
In stirring the sand milling dispersion machine, add 25 kilograms of methyl phenyl silicone resins and 8 kilograms of YLENE, agitating resin is uniformly dispersed in solvent.To wherein adding 30 kilograms of glass powder with low melting point, 2 kilograms of hollow glass microballoons, 10 kilograms of white titanium pigments, 10 kilograms of talcum powder, 12 kilograms of mica powders and 2 kilograms of organobentonites, dispersed with stirring 4 h respectively.Add 1 kilogram of KH-550 sand milling 2 h again, filter the coating that gets product.
With prepared coating be coated on oil removing, rust cleaning and the stainless steel plate handled with YLENE in advance on, do solid work brushing second road, back, coating thickness is controlled at about 50 μ m.Treat to carry out resistance toheat, resistance to impact shock, sticking power test and erosion resistance test behind the curing of coating, the result sees table 1.
Table 1: methyl phenyl silicone resin based high-temp-resistant coating film performance test
| Embodiment | 1000℃/10h | Sticking power | Resistance to salt water/d | Resistance to impact shock/㎏ ㎝ |
| Embodiment 1 | The complete nondiscoloration of filming, the part peeling that ftractures | 1 grade | 7 | ＞50 |
| Embodiment 2 | It is complete to film, and does not dark yellowly ftracture, non-scale | 1 grade | 5 | ＞50 |
| Embodiment 3 | It is complete to film, and the peeling that partly ftractures turns to be yellow at the edge | 1 grade | 9 | ＞50 |
| Embodiment 4 | The complete nondiscoloration of filming is not ftractureed, non-scale | 1 grade | 18 | ＞50 |
| Embodiment 5 | The complete nondiscoloration of filming is not ftractureed, non-scale | 1 grade | 18 | ＞50 |
| Embodiment 6 | The complete nondiscoloration of filming is not ftractureed, non-scale | 1 grade | 16 | ＞50 |
| Embodiment 7 | The complete nondiscoloration of filming is not ftractureed, non-scale | 1 grade | 18 | ＞50 |
Claims (5)
1. methyl phenyl silicone resin based high-temp-resistant coating is characterized in that being prepared from following weight percent proportion raw material:
Methyl phenyl silicone resin: 20 ~ 40 parts,
High-temperature resisting pigment pigment: 5 ~ 30 parts,
Filler: 35 ~ 50 parts,
Auxiliary agent: 1 ~ 5 part,
Solvent is an amount of: 5 ~ 16 parts.
2. a kind of methyl phenyl silicone resin based high-temp-resistant coating according to claim 1 is characterized in that being prepared from following weight percent proportion raw material:
Methyl phenyl silicone resin: 25 ~ 35 parts,
High-temperature resisting pigment: 10 ~ 25 parts,
Filler: 40 ~ 45 parts,
Auxiliary agent: 3 parts,
Solvent is an amount of: 5 ~ 16 parts.
3. wherein said high-temperature resisting pigment is a white titanium pigment.
4. a kind of methyl phenyl silicone resin based high-temp-resistant coating according to claim 1 and 2 is characterized in that wherein said filler is one or more of mica powder, talcum powder, glass powder with low melting point or hollow glass microballoon,
Wherein said auxiliary agent be organobentonite or KH-550 one or both,
Wherein said solvent is YLENE or toluene; Or the mixed solvent of toluene and YLENE.
5. a kind of methyl phenyl silicone resin based high-temp-resistant coating according to claim 1 and 2; It is characterized in that carrying out according to following step: with the methyl phenyl silicone resin is base-material, under the normal temperature, after resin is uniformly dispersed in solvent; Add high-temperature resisting pigment and filler; Grind 2 h at skin grinder, add auxiliary agent again, filter the coating that gets product.
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Application publication date: 20120718 |