CN106085151B - A kind of high tenacity ceramic coating and preparation method thereof - Google Patents

A kind of high tenacity ceramic coating and preparation method thereof Download PDF

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CN106085151B
CN106085151B CN201610435837.8A CN201610435837A CN106085151B CN 106085151 B CN106085151 B CN 106085151B CN 201610435837 A CN201610435837 A CN 201610435837A CN 106085151 B CN106085151 B CN 106085151B
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ceramic coating
high tenacity
resin
tenacity ceramic
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CN106085151A (en
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钱涛
徐凯
刘海兵
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Hangzhou Jihua Polymer Materials Co Ltd
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Hangzhou Jihua Polymer Materials Co Ltd
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    • C09D181/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur, with or without nitrogen, oxygen, or carbon only; Coating compositions based on polysulfones; Coating compositions based on derivatives of such polymers
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Abstract

The present invention relates to field of new materials, the more particularly to preparation of functional high molecule material and applied technical field.Disclose a kind of high tenacity ceramic coating and preparation method thereof.Wherein component of the coating including following parts by weight is made：50 ~ 100 parts of organic resin, 50 ~ 100 parts of silane coupler, 100 ~ 200 parts of alkoxide, 50 ~ 100 parts of filler, 50 ~ 100 parts of pigment, 5 ~ 10 parts of pH adjusting agent, 50 ~ 100 parts of organic solvent, 10 ~ 20 parts of water.The coating that coating of the present invention is formed has high rigidity（≥6H）, high temperature resistant, pliability, excellent adhesive force, the performance such as impact resistance.

Description

A kind of high tenacity ceramic coating and preparation method thereof
Technical field
The present invention relates to field of new materials, the more particularly to preparation of functional high molecule material and applied technical field.
Background technology
Ceramic coating is mostly that the inorganic-organic hybrid of metal oxide, nonmetal oxide and silane coupler composition applies Expect, the coating after film forming has high rigidity using inorganic network as skeleton（Pencil hardness >=6H）, mar-resistance is good, high-temperature resistant, The advantages that non-ignitable, because the physics of film, chemical property are similar to ceramics, therefore it is referred to as " ceramic coating ".Ceramics apply in recent years Expect that industrialization and commercialization in fields such as chemical anticorrosion, aviation, automobile, cooking apparatus are more and more obvious with trend, it grinds Study carefully work turns into the focus to receive much concern.Although ceramic coating has the performance that it is protruded, many technology bottles still be present Neck, such as：Fragility is big, poor toughness, thick film are easy to crack；Pre-treatment to metal base requires higher, bad to adhesive force on base material Deng these technical bottlenecks constrain the further development of ceramic coating industry.
Flexible ceramic coating product in the market, be that ceramic powder is dispersed in organic resin mostly, with high rigidity, Corrosion-resistant, wear-resisting filler fills organic resin, is such as used for petroleum pipeline, the flexible ceramic coating of submerged pipeline, not only Transporting resistance can also be substantially reduced with the abrasion of impedance solid material.CN10107430B describes a kind of the soft of two-component Property ceramic coating, using ceramic powder be scattered in epoxy resin preparation, its hardness of film is 4H, and film is complete after impact is tested It is whole.The A of CN 104140750 describe a kind of high-strength energy-saving crane span structure flexible ceramic coating, and prepared film has fabulous Adhesive force, impact resistance, pliability.However, this flexible ceramic coating is low relative to ceramic coating hardness, scratch resistance It is relative poor.Therefore from the strict sense for, this kind of product can not be referred to as ceramic coating.
The content of the invention
To solve the problems, such as existing ceramic coating poor toughness, poor impact resistance, the invention provides a kind of high tenacity ceramics Coating and preparation method thereof, the present invention be on the basis of the performances such as existing ceramic coating high rigidity, damage resistant, high temperature resistant, it is right A kind of high-performance coating that its pliability, impact resistance are prepared after being improved.Obtained coating has high rigidity（≥ 6H）, high temperature resistant, pliability, excellent adhesive force, the performance such as impact resistance.
The present invention concrete technical scheme be：A kind of high tenacity ceramic coating, including the component of following parts by weight are made：
50 ~ 100 parts of organic resin,
50 ~ 100 parts of silane coupler,
100 ~ 200 parts of alkoxide,
50 ~ 100 parts of filler,
50 ~ 100 parts of pigment,
5 ~ 10 parts of pH adjusting agent,
50 ~ 100 parts of organic solvent,
10 ~ 20 parts of water.
Preferably, described organic resin is selected from silicone modified polyester resin, polyethersulfone resin, polyimides tree One or more in fat, polyamide-imide resin, epoxy silicone resin, organic-silicon-modified focus ratio.
Preferably, the molecular weight of the organic-silicon-modified focus ratio is 150,000 ~ 200,000.Focus ratio need not Curing agent is curable.Focus ratio is poly- good water resistance, wearability, resistance to shrinkage, and it is attached can to improve ceramic coating Put forth effort the shortcomings that poor.The focus ratio of the molecular weight ranges is good with other ingredient compatibilitys, and mobility is moderate, caking property It is good.
Preferably, described silane coupler is selected from MTMS, phenyltrimethoxysila,e, γ-contracting One or more in water glycerine ether oxygen propyl trimethoxy silicane.
Preferably, the one kind or several of described alkoxide in tetraethyl orthosilicate, methyl silicate, butyl titanate Kind.
Preferably, described filler is selected from fumed silica, silicon powder, carborundum, potassium titanate crystal whisker, oxidation It is one or more of in aluminium, mica powder.Further preferably, described filler be selected from fumed silica, silicon powder, carborundum, One or more in aluminum oxide.
Preferably, described pigment is a kind of in titanium dioxide, carbon black, iron oxide red, titanium yellow, cobalt titanate green, cobalt blue It is or several.
Preferably, the one kind of described pH conditioning agents in 10wt% aqueous hydrochloric acid solutions, 20wt% aqueous acetic acids It is or several.
Preferably, described organic solvent is in isopropanol, n-butanol, ethylene glycol monobutyl ether, 1-METHYLPYRROLIDONE One or more.Further preferably, one or more of the solvent in isopropanol, n-butanol, ethylene glycol monobutyl ether.
A kind of preparation method of above-mentioned high tenacity ceramic coating, comprises the following steps：
First by silane coupler, alkoxide, organic solvent is well mixed obtains mixed solution, then organic resin is added to mixed Close in solution, after abundant dissolving, add water and pH adjusting agent, then at 30 ~ 60 DEG C, react 3 ~ 5 hours, reaction terminates cold But after, compound resin is filtrated to get, then pigment, filler are added in compound resin, 3 ~ 5h, filtering are ground in grinder Discharging obtains high tenacity ceramic coating.
The present invention forms organic matter/nothing by using special hybrid mode by sol-gel process Machine thing inierpeneirating network structure, i.e., alkoxide is added in organic polymer as precursor, precursor is after hydrolysis in organic polymer Thing molecular structure situ generates inorganic network, and compared with conventional method, the dispersiveness of organic matter and inorganic matter is more preferable, to avoid Consistency problem caused by phase separation, film can be made in high rigidity（≥6H）, heat-resisting quantity it is good on the premise of, while assign it The performances such as high-flexibility, excellent adhesive force, high-impact, there is higher application value.
It is compared with the prior art, the beneficial effects of the invention are as follows：
（1）The hardness that coating is prepared in the present invention is high（≥6H）, high temperature resistant, pliability is good, adhesive force is good, impact resistance （50cm*kg films are complete）.
（2）Relative to existing ceramic coating, coating operations of the invention are easy（One-component, without curing）, the holding time Longer, the pre-treatment to base material requires low（Can be without blasting treatment）.
Embodiment
With reference to embodiment, the invention will be further described.It is raw materials used commercially available or can adopt in embodiment It is prepared with conventional method, the number is parts by weight.
1. the method for testing in detection method：
1）Pencil hardness：GB/T 6739-2006
2）Adhesive force：GB/T 9286-1998
3）Impact resistance：GB/T 1732-1993
2. the preparation method of coating：
Sprayed, dried 10 minutes in 280 DEG C of baking ovens, obtaining thickness is on the aluminium sheet of sandblasting with high tenacity ceramic coating 35 microns of film.
Embodiment 1
（1）Organic resin：50 parts of silicone modified polyester resin,
Silane coupler：50 parts of phenyl trimethoxy,
Alkoxide：100 parts of tetraethyl orthosilicate,
Filler：10 parts of potassium titanate crystal whisker, 20 parts of silicon powder, 20 parts of aluminum oxide,
Pigment：50 parts of titanium dioxide,
PH adjusting agent：5 parts of 10wt% aqueous hydrochloric acid solutions,
Organic solvent：50 parts of isopropanol,
10 parts of deionized water.
（2）First phenyltrimethoxysila,e, tetraethyl orthosilicate, isopropanol are well mixed and obtain mixed solution, then will be had Machine silicon-modified polyester resin is added in mixed solution, and stirring adds deionized water and 10wt% hydrochloric acid is water-soluble after abundant dissolving Liquid, then at 30 DEG C, stir 5 hours, after cooling, be filtrated to get compound resin.Then, by potassium titanate crystal whisker, silicon powder, Aluminum oxide, titanium dioxide are added in compound resin, after grinding 4h in grinder, are filtrated to get high tenacity with 250 mesh filter screens and are made pottery Porcelain coating 1.
Embodiment 2
（1）Organic resin：100 parts of silicone modified polyester resin,
Silane coupler：50 parts of phenyltrimethoxysila,e, 50 parts of γ-glycidyl ether oxygen propyl trimethoxy silicane,
Alkoxide：100 parts of tetraethyl orthosilicate, 100 parts of butyl titanate,
Filler：40 parts of carborundum, 40 parts of silicon powder, 20 parts of aluminum oxide,
Pigment：70 parts of carbon black, 20 parts of titanium yellow, 10 parts of cobalt titanate green,
PH adjusting agent：10 parts of 20wt% aqueous acetic acids,
Organic solvent：50 parts of isopropanol, 50 parts of normal propyl alcohol,
20 parts of deionized water.
（2）First by phenyltrimethoxysila,e, γ-glycidyl ether oxygen propyl trimethoxy silicane, tetraethyl orthosilicate, different Propyl alcohol, n-butanol are well mixed to obtain mixed solution, then silicone modified polyester resin is added in mixed solution, treats fully After dissolving, 20wt% aqueous acetic acids, deionized water are added, then at 60 DEG C, stirs 5 hours, after cooling, is filtrated to get Compound resin.Then, carborundum, silicon powder, aluminum oxide, carbon black, titanium yellow, cobalt titanate green are added in compound resin, ground After grinding 3h in grinding machine, high tenacity ceramic coating 2 is filtrated to get with 250 mesh filter screens.
Embodiment 3
（1）Organic resin：50 parts of polyamide-imide resin, 50 parts of polyethersulfone resin,
Silane coupler：50 parts of phenyltrimethoxysila,e, 50 parts of MTMS,
Alkoxide：200 parts of methyl silicate,
Filler：20 parts of mica powder, 40 parts of silicon powder, 40 parts of aluminum oxide,
Pigment：100 parts of iron oxide red,
PH adjusting agent：10 parts of 20wt% aqueous acetic acids,
Organic solvent：100 parts of 1-METHYLPYRROLIDONE,
20 parts of deionized water.
（2）First phenyltrimethoxysila,e, MTMS, methyl silicate, 1-METHYLPYRROLIDONE are mixed Conjunction uniformly obtains mixed solution, then polyamide-imide resin, polyethersulfone resin are added in mixed solution, treats fully to dissolve Afterwards, 20wt% aqueous acetic acids, deionized water are added, then at 60 DEG C, stirs 3 hours, after cooling, is filtrated to get compound Resin.Then, mica powder, silicon powder, aluminum oxide, iron oxide red are added in compound resin, after grinding 5h in grinder, High tenacity ceramic coating 3 is filtrated to get with 250 mesh filter screens.
Embodiment 4
（1）Organic resin：80 parts of silicone modified polyester resin, 20 parts of epoxy silicone resin,
Silane coupler：100 parts of phenyltrimethoxysila,e,
Alkoxide：200 parts of tetraethyl orthosilicate,
Filler：10 parts of fumed silica, 40 parts of silicon powder, 50 parts of aluminum oxide,
Pigment：80 parts of titanium dioxide, 20 parts of cobalt blue,
PH adjusting agent：5 parts of 10wt% aqueous hydrochloric acid solutions,
Solvent：50 parts of isopropanol, 50 parts of ethylene glycol monobutyl ether,
20 parts of deionized water.
（2）First phenyltrimethoxysila,e, tetraethyl orthosilicate, isopropanol, ethylene glycol monobutyl ether are mixed Solution is closed, then silicone modified polyester resin, epoxy silicone resin are added in mixed solution, after abundant dissolving, is added Enter 10wt% aqueous hydrochloric acid solutions, deionized water, then at 30 DEG C, stir 5 hours, after cooling, be filtrated to get compound resin. Then, fumed silica, silicon powder, aluminum oxide, titanium dioxide, cobalt blue are added in compound resin, ground in grinder After grinding 4h, high tenacity ceramic coating 4 is filtrated to get with 250 mesh filter screens.
Embodiment 5
（1）Organic resin：50 parts of polyimide resin,
Silane coupler：50 parts of γ-glycidyl ether oxygen propyl trimethoxy silicane,
Alkoxide：200 parts of tetraethyl orthosilicate,
Filler：10 parts of fumed silica, 20 parts of silicon powder, 20 parts of aluminum oxide,
Pigment：50 parts of iron oxide red,
PH adjusting agent：5 parts of 10wt% aqueous hydrochloric acid solutions,
Organic solvent：50 parts of 1-METHYLPYRROLIDONE,
10 parts of deionized water.
（2）First γ-glycidyl ether oxygen propyl trimethoxy silicane, tetraethyl orthosilicate, 1-METHYLPYRROLIDONE are mixed Mixed solution uniformly is obtained, then silicone modified polyester resin is added in mixed solution, after abundant dissolving, is added 10wt% aqueous hydrochloric acid solutions, deionized water, then at 30 DEG C, stir 5 hours, after cooling, be filtrated to get compound resin.So Afterwards, fumed silica, silicon powder, aluminum oxide, iron oxide red are added in compound resin, 4h is ground in grinder Afterwards, it is filtrated to get high tenacity ceramic coating 5 with 250 mesh filter screens.
Embodiment 6
（1）Organic resin：50 parts of silicone modified polyester resin,
Silane coupler：50 parts of phenyltrimethoxysila,e,
Alkoxide：100 parts of tetraethyl orthosilicate,
Filler：SiC30 parts, 10 parts of silicon powder, 10 parts of aluminum oxide,
Pigment：50 parts of carbon black,
PH adjusting agent：5 parts of 10wt% aqueous hydrochloric acid solutions,
Organic solvent：50 parts of isopropanol,
10 parts of deionized water.
（2）First phenyltrimethoxysila,e, tetraethyl orthosilicate, isopropanol are well mixed and obtain mixed solution, then will be had Machine silicon-modified polyester resin is added in mixed solution, after abundant dissolving, adds 10wt% aqueous hydrochloric acid solutions, deionized water, so Afterwards at 30 DEG C, stir 5 hours, after cooling, be filtrated to get compound resin.Then, by carborundum, silicon powder, aluminum oxide, charcoal It is black to be added in compound resin, after grinding 4h in grinder, high tenacity ceramic coating 6 is filtrated to get with 250 mesh filter screens.
Embodiment 7
（1）Organic resin：50 parts of silicone modified polyester resin, molecular weight are 150,000 ~ 200,000 organic-silicon-modified poly- phenol 25 parts of oxygen tree fat,
Silane coupler：75 parts of phenyltrimethoxysila,e,
Alkoxide：150 parts of tetraethyl orthosilicate,
Filler：10 parts of fumed silica, 40 parts of silicon powder, 25 parts of aluminum oxide,
Pigment：50 parts of titanium dioxide, 25 parts of cobalt blue,
PH adjusting agent：7.5 parts of 10wt% aqueous hydrochloric acid solutions,
Solvent：40 parts of isopropanol, 35 parts of ethylene glycol monobutyl ether,
15 parts of deionized water.
（2）First phenyltrimethoxysila,e, tetraethyl orthosilicate, isopropanol, ethylene glycol monobutyl ether are mixed Solution is closed, then silicone modified polyester resin, machine Si modification focus ratio are added in mixed solution, treats fully to dissolve Afterwards, 10wt% aqueous hydrochloric acid solutions, deionized water are added, then at 45 DEG C, stirs 4 hours, after cooling, is filtrated to get compound Resin.Then, fumed silica, silicon powder, aluminum oxide, titanium dioxide, cobalt blue are added in compound resin, in grinder After middle grinding 4h, high tenacity ceramic coating 7 is filtrated to get with 250 mesh filter screens.
The coating performance testing result of embodiment 1 ~ 7, it is as shown in the table
Detection project Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6 Embodiment 7
Pencil hardness 6H 7H 6H 6H 6H 7H 7H
Adhesive force 0 grade 0 grade 0 grade 0 grade 0 grade 0 grade 0 grade
Impact resistance Pass through Pass through Pass through Pass through Pass through Pass through Pass through
Raw materials used in the present invention, equipment, it is the conventional raw material, equipment of this area unless otherwise noted；In the present invention Method therefor, it is the conventional method of this area unless otherwise noted.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, it is every according to the present invention Any simple modification, change and the equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side The protection domain of case.

Claims (9)

  1. A kind of 1. high tenacity ceramic coating, it is characterised in that：Component including following parts by weight is made：
    50 ~ 100 parts of organic resin,
    50 ~ 100 parts of silane coupler,
    100 ~ 200 parts of alkoxide,
    50 ~ 100 parts of filler,
    50 ~ 100 parts of pigment,
    5 ~ 10 parts of pH adjusting agent,
    50 ~ 100 parts of organic solvent,
    10 ~ 20 parts of water；
    The preparation method of described high tenacity ceramic coating comprises the following steps：
    First by silane coupler, alkoxide, organic solvent is well mixed obtains mixed solution, then that organic resin is added into mixing is molten In liquid, after abundant dissolving, water and pH adjusting agent are added, then at 30 ~ 60 DEG C, is reacted 3 ~ 5 hours, reaction terminates cooling Afterwards, compound resin is filtrated to get, then pigment, filler are added in compound resin, 3 ~ 5h is ground in grinder, is filtered out Material obtains high tenacity ceramic coating.
  2. 2. a kind of high tenacity ceramic coating according to claim 1, it is characterised in that described organic resin is selected from organic Silicon-modified polyester resin, polyethersulfone resin, polyimide resin, polyamide-imide resin, epoxy silicone resin, organosilicon One or more in modified focus ratio.
  3. A kind of 3. high tenacity ceramic coating according to claim 2, it is characterised in that the organic-silicon-modified poly phenol oxygen tree The molecular weight of fat is 150,000 ~ 200,000.
  4. 4. a kind of high tenacity ceramic coating according to claim 1, it is characterised in that described silane coupler is selected from first Base trimethoxy silane, phenyltrimethoxysila,e, one kind in γ-glycidyl ether oxygen propyl trimethoxy silicane or several Kind.
  5. 5. a kind of high tenacity ceramic coating according to claim 1, it is characterised in that described alkoxide is selected from positive silicic acid second One or more in ester, methyl silicate, butyl titanate.
  6. 6. a kind of high tenacity ceramic coating according to claim 1, it is characterised in that described filler is selected from vapor phase method two It is one or more of in silica, silicon powder, carborundum, potassium titanate crystal whisker, aluminum oxide, mica powder.
  7. A kind of 7. high tenacity ceramic coating according to claim 1, it is characterised in that described pigment be selected from titanium dioxide, It is one or several kinds of in carbon black, iron oxide red, titanium yellow, cobalt titanate green, cobalt blue.
  8. 8. a kind of high tenacity ceramic coating according to claim 1, it is characterised in that described pH conditioning agents are selected from One or more in 10wt% aqueous hydrochloric acid solutions, 20wt% aqueous acetic acids.
  9. 9. a kind of high tenacity ceramic coating according to claim 1, it is characterised in that described organic solvent is isopropyl One or more in alcohol, n-butanol, ethylene glycol monobutyl ether, 1-METHYLPYRROLIDONE.
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