CN103451641A - Modified silanized metal surface pretreatment agent containing diphenylethyl diphenol polyoxyethylene ether and preparation method thereof - Google Patents
Modified silanized metal surface pretreatment agent containing diphenylethyl diphenol polyoxyethylene ether and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a modified silanized metal surface pretreatment agent containing diphenylethyl diphenol polyoxyethylene ether. The pretreatment agent is prepared from the following raw materials in parts by weight: 100 parts of deionized water, 10-15 parts of modified coupling agent, 10-15 parts of ethanol, 30-40 parts of gamma-chloropropyl triethoxysilane, 20-30 parts of gamma-glycidyloxypropyl trimethoxysilane, 1-2 parts of dicumyl peroxide, 0.002-0.003 part of perfluorooctyl sodium sulfonate, 0.3-0.5 part of wood ash, 4-6 parts of acrylic emulsion, 2-3 parts of sodium carboxymethyl cellulose, 0.4-1.0 part of Span80, 0.2-0.6 part of diphenylethyl diphenol polyoxyethylene ether, 0.005-0.01 part of lanthanum acetate and 0.1-0.3 part of phytic acid. A final product is obtained by modifying the coupling agent, compounding, adding auxiliaries and carrying out distribution, mixing and reaction. The modified silanized surface pretreatment agent has the characteristics of no toxicity, environment friendliness, convenience in use, compact and uniform silane film, strong adhesion and good corrosion resistance.
Description
Technical field
The present invention relates to the metal conditioner technology, be specifically related to a kind of modified silicon alkanisation metallic surface pretreating reagent containing hexichol ethyl biphenyl phenol polyethenoxy ether and preparation method thereof.
Background technology
The corrosion of metallic substance all occurs all the time around us.Annual according to statistics approximately have 10% metallic substance can't reclaim for corrosion, this not only causes the huge waste of metals resources, also normal production and personnel safety are brought to serious threat, it is a kind of anti-corrosion method commonly used that metallic substance is carried out to surface treatment, for coated metal pre-treatment main method, is parco-lubrizing at present.Environment is had to the problems such as pollution but traditional metal surface treating method exists because containing hazardous and noxious substances, be not suitable for the environmental requirement that human society is more and more higher.
Metallic substance, after phosphatization, can strengthen the sticking power between metallic matrix and coating, improves corrosion resistance nature.Bonderizing no doubt has plurality of advantages, but also there is the drawback that much himself can't overcome: all contain the objectionable impuritiess such as phosphoric acid salt and heavy metal in etching solution, and all more or less can produce sediment and obnoxious flavour in treating processes, what impact was produced normally carries out, and the waste water COD of discharge and heavy metal will endanger environment if do not advanced environmental protection treatment; In addition, the bonderizing major part need be carried out under the condition of heating, and energy consumption is larger, complex process, and operation is also inconvenient.Along with social development and progress, people are also more and more high to the requirement of coated metal prefinished products, not only wish that its self performance is good, more wish that it can meet growing environmental protection needs, HUMAN HEALTH requires and the resources conservation requirement.These drawbacks that conventional phosphatizing is processed are just seriously restricting further developing and applying of it.So people hope and can develop a kind of brand-new treatment process, when it can keep conventional phosphatizing treatment process advantage, can accomplish that again technique is simple, environmental protection, comprehensive cost is low.
Silanization is processed to compare with conventional phosphatizing has following a plurality of advantage: without the harmful heavy metal ion, not phosphorous, and without heating.The silane treatment process does not produce sediment, and the treatment time is short, controls easy.Treatment step is few, can save table and adjust operation, and tank liquor is reusable.Effectively improve the sticking power of paint to base material.But the multiple base materials such as collineation processing iron plate, galvanized sheet, aluminium sheet.But with regard to current domestic technique, not very ripe, especially, on the type selecting of silane and auxiliary agent, also have a lot of not enough places.
Metallic surface silanization is processed and is had broad application prospects, but the silane film that prior art becomes exists, corrosion resistance is not strong, film forming is inhomogeneous, do not possess the defects such as " selfreparing " performance or " selfreparing " poor performance, has limited its development.
Summary of the invention
The invention discloses a kind of modified silicon alkanisation metallic surface pretreating reagent containing hexichol ethyl biphenyl phenol polyethenoxy ether and preparation method thereof.
The technical solution used in the present invention is as follows:
A kind of modified silicon alkanisation metallic surface pretreating reagent containing hexichol ethyl biphenyl phenol polyethenoxy ether, it is characterized in that, feed composition by following weight part is made: deionized water 100, modification coupling agent 10-15, ethanol 10-15, γ-chloropropyl triethoxysilane 30-40, γ-glycidyl ether oxygen propyl trimethoxy silicane 20-30, dicumyl peroxide 1-2, perfluoro octyl sulfonic acid sodium 0.002-0.003, trees ash 0.3-0.5, ACRYLIC EMULSION 4-6, Xylo-Mucine 2-3, sorbester p17 0.4-1.0, hexichol ethyl biphenyl phenol polyethenoxy ether 0.2-0.6, lanthanum acetate 0.005-0.01, phytic acid 0.1-0.3.
Described a kind of modified silicon alkanisation metallic surface pretreating reagent containing hexichol ethyl biphenyl phenol polyethenoxy ether, it is characterized in that, feed composition by following weight part is made: deionized water 100, modification coupling agent 12, ethanol 14, γ-glycidyl ether oxygen propyl trimethoxy silicane 25, γ-chloropropyl triethoxysilane 35, dicumyl peroxide 1.5, Sodium perfluorooctanoate 0.0024, trees ash 0.4, ACRYLIC EMULSION 5, Xylo-Mucine 2, sorbester p17 0.6, hexichol ethyl biphenyl phenol polyethenoxy ether 0.4, lanthanum acetate 0.007, phytic acid 0.25.
The preparation method of the described modified silicon alkanisation metallic surface pretreating reagent containing hexichol ethyl biphenyl phenol polyethenoxy ether, is characterized in that, comprises the following steps:
(1) modification coupling agent preparation
The water-soluble nano grade silica sol is added to 4-5% nano zinc powder, 3-5% ferric oxide, 4-6%2-aminoethyl 17 alkenyl imidazolines, be mixed and heated to 95-115 ℃, cooling getting final product after 20-30 minute;
(2) first add γ-glycidyl ether oxygen propyl trimethoxy silicane by the formula rate amount in stirring tank, then add dicumyl peroxide, after stirring 3-4 minute with the speed of 300-400rpm, add again γ-chloropropyl triethoxysilane, after stirring 3-5 minute with the speed of 300-400rpm, Sodium perfluorooctanoate and trees ash are added wherein, at room temperature with the condition of protection of inert gas under, speed with 350-450rpm stirs 30-40 minute again, obtains built up silane couple A;
(3) by formula rate, deionized water is injected to stirring tank, the modification coupling agent under whipped state, step (1) made adds in still, stir after 1-2 minute, add again ethanol, continue to stir after 2-3 minute, then add ACRYLIC EMULSION, stir 5-6 minute, obtain mixing solutions B, stirring velocity is 2000～2500rpm;
(4) A and B are mixed, then add successively Xylo-Mucine, sorbester p17, hexichol ethyl biphenyl phenol polyethenoxy ether, phytic acid, under whipped state, isothermal reaction under 55-65 ℃ of condition, obtain mixed solution C;
(5) finally add lanthanum acetate, stir after 10-15 minute, filter and obtain the finished product.
Use temperature: normal temperature, treatment time: 3～6 minutes (drill traverse) 1～3 minute (spray);
Working fluid pH value: 4.5-5.5, working concentration: 4-5%.
Beneficial effect of the present invention:
The modification of the present invention by coupling agent and composite, overcome in the prior art silane film and had that corrosion resistance is strong, the inhomogeneous shortcoming of film forming, the present invention is by regulating formula materials, improve preparation technology, the agent of resulting modified silicon alkanisation surface pretreatment, have characteristics nontoxic, environmental protection, in metallic surface, formed silane film corrosion resistance is strong, film is fine and close evenly, strong adhesion, produce without the dust phenomenon, is widely used in the pre-treatment of the spraying paint that dusts of various metallic surfaces.
Embodiment
Embodiment 1
Take raw material (kg) by following weight: deionized water 100, modification coupling agent 12, ethanol 14, γ-glycidyl ether oxygen propyl trimethoxy silicane 25, γ-chloropropyl triethoxysilane 35, dicumyl peroxide 1.5, Sodium perfluorooctanoate 0.0024, trees ash 0.4, ACRYLIC EMULSION 5, Xylo-Mucine 2, sorbester p17 0.6, hexichol ethyl biphenyl phenol polyethenoxy ether 0.4, lanthanum acetate 0.007, phytic acid 0.25
The preparation method:
(1) modification coupling agent preparation
The water-soluble nano grade silica sol is added to 4-5% nano zinc powder, 3-5% ferric oxide, 4-6%2-aminoethyl 17 alkenyl imidazolines, be mixed and heated to 95-115 ℃, cooling getting final product after 20-30 minute;
(2) first add γ-glycidyl ether oxygen propyl trimethoxy silicane by the formula rate amount in stirring tank, then add dicumyl peroxide, after stirring 3-4 minute with the speed of 300-400rpm, add again γ-chloropropyl triethoxysilane, after stirring 3-5 minute with the speed of 300-400rpm, Sodium perfluorooctanoate and trees ash are added wherein, at room temperature with the condition of protection of inert gas under, speed with 350-450rpm stirs 30-40 minute again, obtains built up silane couple A;
(3) by formula rate, deionized water is injected to stirring tank, the modification coupling agent under whipped state, step (1) made adds in still, stir after 1-2 minute, add again ethanol, continue to stir after 2-3 minute, then add ACRYLIC EMULSION, stir 5-6 minute, obtain mixing solutions B, stirring velocity is 2000～2500rpm;
(4) A and B are mixed, then add successively Xylo-Mucine, sorbester p17, hexichol ethyl biphenyl phenol polyethenoxy ether, phytic acid, under whipped state, isothermal reaction under 55-65 ℃ of condition, obtain mixed solution C;
(5) finally add lanthanum acetate, stir after 10-15 minute, filter and obtain the finished product.
The property indices of the silanized surface pretreating reagent that modified silicon alkanisation surface pretreatment agent of the present invention and prior art are produced contrasts as following table:
| Project | Implement 1 | Prior art |
| Outward appearance | Colourless | Colourless |
| Treatment time min | 4 | ? 20 |
| Treatment temp ℃ | Normal temperature | 140 |
| Post-treatment condition | Pure water is washed | First pickling, washing with water |
| Tank liquor pH value | 5.0 | 9.0 |
| Silane film | Evenly fine and close | Rete is inhomogeneous |
There are energy-saving and environmental protection when silanization protective agent for surface treatment of the present invention is processed metal works as can be seen from the table, the characteristics that effect is high, silane film is evenly fine and close simultaneously.
Claims (3)
1. the modified silicon alkanisation metallic surface pretreating reagent containing hexichol ethyl biphenyl phenol polyethenoxy ether, it is characterized in that, feed composition by following weight part is made: deionized water 100, modification coupling agent 10-15, ethanol 10-15, γ-chloropropyl triethoxysilane 30-40, γ-glycidyl ether oxygen propyl trimethoxy silicane 20-30, Sodium perfluorooctanoate 0.001-0.004, trees ash 0.3-0.5, ACRYLIC EMULSION 4-6, Xylo-Mucine 2-3, sorbester p17 0.4-1.0, hexichol ethyl biphenyl phenol polyethenoxy ether 0.2-0.5, lanthanum acetate 0.005-0.01, phytic acid 0.1-0.3.
2. a kind of modified silicon alkanisation metallic surface pretreating reagent containing hexichol ethyl biphenyl phenol polyethenoxy ether according to claim 1, it is characterized in that, feed composition by following weight part is made: deionized water 100, modification coupling agent 12, ethanol 14, γ-glycidyl ether oxygen propyl trimethoxy silicane 25, γ-chloropropyl triethoxysilane 35, dicumyl peroxide 1.5, Sodium perfluorooctanoate 0.0026, trees ash 0.4, ACRYLIC EMULSION 5, Xylo-Mucine 2, sorbester p17 0.6, hexichol ethyl biphenyl phenol polyethenoxy ether 0.4, lanthanum acetate 0.007, phytic acid 0.25.
3. the preparation method of the modified silicon alkanisation metallic surface pretreating reagent containing hexichol ethyl biphenyl phenol polyethenoxy ether as claimed in claim 1 or 2, is characterized in that, comprises the following steps:
(1) modification coupling agent preparation
The water-soluble nano grade silica sol is added to 4-5% nano zinc powder, 3-5% ferric oxide, 4-6%2-aminoethyl 17 alkenyl imidazolines, be mixed and heated to 95-115 ℃, cooling getting final product after 20-30 minute;
(2) first add γ-glycidyl ether oxygen propyl trimethoxy silicane by the formula rate amount in stirring tank, then add dicumyl peroxide, after stirring 3-4 minute with the speed of 300-400rpm, add again γ-chloropropyl triethoxysilane, after stirring 3-5 minute with the speed of 300-400rpm, Sodium perfluorooctanoate and trees ash are added wherein, at room temperature with the condition of protection of inert gas under, speed with 350-450rpm stirs 30-40 minute again, obtains built up silane couple A;
(3) by formula rate, deionized water is injected to stirring tank, the modification coupling agent under whipped state, step (1) made adds in still, stir after 1-2 minute, add again ethanol, continue to stir after 2-3 minute, then add ACRYLIC EMULSION, stir 5-6 minute, obtain mixing solutions B, stirring velocity is 2000～2500rpm;
(4) A and B are mixed, then add successively Xylo-Mucine, sorbester p17, hexichol ethyl biphenyl phenol polyethenoxy ether, phytic acid, under whipped state, isothermal reaction under 55-65 ℃ of condition, obtain mixed solution C;
(5) finally add lanthanum acetate, stir after 10-15 minute, filter and obtain the finished product.
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| JP2020529497A (en) * | 2017-07-31 | 2020-10-08 | ノベリス・インコーポレイテッドＮｏｖｅｌｉｓ Ｉｎｃ． | Pretreatment compositions, coated aluminum alloys, and how to make them |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102977774A (en) * | 2012-12-04 | 2013-03-20 | 安徽省宿州市龙华机械制造有限公司 | Modified silane surface pretreating agent containing polyoxyethylene octadecanol ether and preparation method of modified silane surface pretreating agent |
| CN102993870A (en) * | 2012-12-04 | 2013-03-27 | 安徽省宿州市龙华机械制造有限公司 | Modified silanized metal surface pre-treating agent containing polyoxyethylene oleate and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977774A (en) * | 2012-12-04 | 2013-03-20 | 安徽省宿州市龙华机械制造有限公司 | Modified silane surface pretreating agent containing polyoxyethylene octadecanol ether and preparation method of modified silane surface pretreating agent |
| CN102993870A (en) * | 2012-12-04 | 2013-03-27 | 安徽省宿州市龙华机械制造有限公司 | Modified silanized metal surface pre-treating agent containing polyoxyethylene oleate and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020529497A (en) * | 2017-07-31 | 2020-10-08 | ノベリス・インコーポレイテッドＮｏｖｅｌｉｓ Ｉｎｃ． | Pretreatment compositions, coated aluminum alloys, and how to make them |
| US11519076B2 (en) | 2017-07-31 | 2022-12-06 | Novelis Inc. | Pretreatment compositions, coated aluminum alloys, and methods of making the same |
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Application publication date: 20131218 |