CN101168645A - Transparent organic silicon rigidity-increasing dope - Google Patents
Transparent organic silicon rigidity-increasing dope Download PDFInfo
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- CN101168645A CN101168645A CNA2006100539506A CN200610053950A CN101168645A CN 101168645 A CN101168645 A CN 101168645A CN A2006100539506 A CNA2006100539506 A CN A2006100539506A CN 200610053950 A CN200610053950 A CN 200610053950A CN 101168645 A CN101168645 A CN 101168645A
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Abstract
The invention discloses transparent organosilicon hard coating, in particular to organosilicon resin coating material which can form cementing excellent hard and compactness, and transparent and smooth coating with basis material after the basis material is used. Under the normal temperature, methyl tertiary alkane oxygen radical, silicon latex solution, polymerization catalyst and water are added in a reaction vessel according to certain scale, and mixed continuously and reacted for 10 to 50 hours until reaction liquid becomes homogeneous phase, and then the organosilicon resin condensation polymer is manufactrued. After condensation polymer solution is filtered, diluting solvent with appropriate amount is added to be mixed equably, and then polyether modified siloxane with appropriate amount is added to be used as surface active agent again, and uniform mixing is performed, thereby, the organosilicon resin hard coating is produced.
Description
Technical field
The present invention relates to a kind of transparent organic silicon rigidity-increasing dope, be meant especially to be applied to the silicone resin coating material that can form behind the base material with base material bonding excellence, hard and compact, transparent bright and clean coating.
Background technology
Transparent organic silicon rigidity-increasing dope is to issue the water white silicone resin solution that unboiled water depolymerizes and reacts and form by the polyfunctional group organosilane monomer in acid catalysis, is a kind of highly cross-linked polysiloxane.Transparent organic silicon rigidity-increasing dope can be used as the hard coat that increases of transparent plasticss such as synthetic glass, polycarbonate, polystyrene, significantly improves its wear-resisting, corrosion-resistant and ageing resistance, and can improve the transmittance of the optical mirror slip made from these materials.Simultaneously, transparent organic silicon rigidity-increasing dope also can be used as the supercoat of all kinds of metal productss, finishing material, stone artifact etc., improves their performances such as wear-resisting, ageing-resistant, corrosion-resistant, water-fast and uvioresistant.
The transparent organic silicon cold coating is a starting raw material with the methyl trialkoxysilane normally, is catalyzer with hydrochloric acid, and heating makes it that hydrolysis condensation reaction take place in ethanol, aqueous systems, thereby make.But the silicone resin coating that this method makes need add curing agent component when solidifying, and so the hardness of film of gained is on the low side, usually has only 2H～3H (pencil hardness); And owing to added solidifying agent, dead glue phenomenon very easily takes place in organosilicon coating at normal temperatures, has shortened the storage time of coating so greatly, brings very big inconvenience to application.
Chinese patent (CN1544560) has reported that be raw material with silicone resin with containing organosilyl polymethacrylate, add an amount of zinc acetate, 160 ℃～180 ℃ following polycondensations, at the linking agent, initiator and the heat-resistant filler that add silicone resin solidifying agent, polyacrylic ester, have higher cohesiveness after the silicone based thermal protection coating that makes at room temperature solidifies, hardness of film increases.But the transparency of filming that this method makes is not high, is difficult for using on transparent plastics.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art existence, thereby a kind of silicone resin coating simple and easy, that cost performance is high of operating is provided, its plated film is used and is solidified transparent bright and clean, the hard wear resistant of coating that the back forms, applied range.
As mentioned above, purpose of the present invention promptly is that a kind of transparent organic silicon rigidity-increasing dope will be provided, after its use, can form and base material bonding excellence, hard and compact, transparent bright and clean coating, and it can form erosion resistance and the resistance to scratch excellence while coating in aspect excellences such as other rerum naturas such as didirtresistance, wear resistance, thermotolerance, static resistances on the surface of various base materials.
In order to achieve the above object, the present invention adds a kind of hard component that increases in the methyl trialkoxysilane hydrolysis condensation reaction, and promptly adopting silicon is that latax prepares.But this silicon is latax uniform distribution in silicone resin, can not reduce the transmittance of silicone resin, thereby makes the silicone resin coating that makes can keep good properties of transparency after using curing.
Concrete implementing process of the present invention is as follows:
Under the normal temperature, be that latax, polymerizing catalyst and water add in the reaction vessel by a certain percentage with methyl trialkoxysilane, silicon, continuously stirring reaction 10～50 hours becomes homogeneous phase up to reaction solution, and this is the silicone resin condensation polymer.This condensation polymer solution is filtered, add an amount of diluting solvent, stir, add an amount of polyether modified siloxane again, mix, so promptly make the silicone resin rigidity-increasing dope as tensio-active agent.
In the foregoing invention technology, used methyl trialkoxysilane mainly is meant methyltrimethoxy silane, Union carbide A-162.
In the foregoing invention technology, used silicon is its SiO of latax
2Content is generally 20%～40%.This silicon is the consumption of latax, generally is 10%～90% of methyl trialkoxysilane weight, and suitable consumption is 25%～75%.
In the foregoing invention technology, used polymerizing catalyst can be organic acid, mineral acid, metal carboxylate, acetylacetonate complex.Organic acid comprises acetate, propionic acid, butyric acid, valeric acid, maleic acid and stearic acid; Mineral acid comprises hydrochloric acid, hydrofluoric acid, nitric acid, sulfuric acid, chloric acid and hydrogen peroxide; Metal carboxylate is with formula (RCOO)
nThe compound that M represents, wherein R represents C
1～22Fat base or alicyclic radical, M are represented Ni, Ti, Pt, Rh, Co, Fe, Ru, Os, Pd, Ir and Al; N is the valency of M; This metal carboxylate can be acid anhydride or hydrate.Acetylacetonate complex is the complex compound that comprises with negatively charged ion acac-coordinate atoms metal.The consumption of polymerizing catalyst generally is 0.001%～10% of a methyl trialkoxysilane weight.
In the foregoing invention technology, used diluting solvent comprises ethanol, Virahol, propyl carbinol.Its consumption generally is 5%～200% of a prepared organic silicone resin condensation polymer weight, and suitable consumption is 25%～150%.
The silicone resin rigidity-increasing dope that the foregoing invention method makes is a kind of highly cross-linked polysiloxane, is to be main chain with Si-O-Si, connects the cross-linking type superpolymer of organic group on the Siliciumatom.The Siliciumatom electronegativity is just low, and it is certain ionic to make the Si-O key have; Si-O-Si bond energy, bond angle are all big than C-C key; And this polysiloxane also comprises the repeat unit structure of Si-H key.This special valence bond structure makes this silicone resin rigidity-increasing dope have many excellent physical chemistry that are different from carbon-based polymer, comprise anti-height stability, wear resistance, ageing resistance, erosion resistance, water tolerance, insulativity, radiation resistance, static resistance and uvioresistant etc., thereby can all obtain to use widely aspect many in motor, electrical equipment, electronics, building, aviation, chemical industry and daily life etc.
The silicone resin rigidity-increasing dope that the foregoing invention method makes can carry out plated film by methods such as spraying, dip-coating, roller coat, vacuum sprayings.After matrix or substrate coated this silicone resin rigidity-increasing dope, the heating baked and cured, solidification value is 50 ℃～80 ℃ usually, 0.5～3 hour set time.The silicone resin that so makes is filmed, and its any surface finish is transparent, hard wear resistant, and pencil hardness can reach 6H～9H.
Embodiment
Transparent organic silicon rigidity-increasing dope of the present invention is described further by following specific embodiment.
Embodiment 1
In being furnished with the 20L four-hole vial of tetrafluoro teeter column, add Union carbide A-162 9.85kg while stirring, silicon is latax 2.46kg, stearic acid 10g and water 0.2kg, in 25 ℃～30 ℃ following continuously stirring reactions 24 hours.With this silicone resin condensation polymer solution secondary filter, add the agent of 5.65kg alcohol dilution, stir; Add tensio-active agent 40g again, mix.Blowing packs.
This silicone resin rigidity-increasing dope through plated film use the coating of solidifying the back gained transparent bright and clean, hard and compact is wear-resisting, pencil hardness reaches 6H above (with Q H Q-A pencil hardness meter by GB GB/T6739-86 method mensuration); Excellent corrosion resistance (the CASS test method(s) is the acetate spraying method that copper quickens).
Embodiment 2
In being furnished with the 20L four-hole vial of tetrafluoro teeter column, add methyltrimethoxy silane 8.78kg while stirring, silicon is latax 4.26kg, aluminum acetate 22g and water 0.2kg, in 25 ℃～30 ℃ following continuously stirring reactions 30 hours.With this silicone resin condensation polymer solution secondary filter, add the agent of 10.65kg isopropanol, stir; Add tensio-active agent 50g again, mix.Blowing packs.
This silicone resin rigidity-increasing dope is after plated film is used curing, and the pencil hardness that records coating reaches more than the 7H; Excellent corrosion resistance.
Embodiment 3
In the 1000L enamel reaction still, adding Union carbide A-162 555kg, silicon were latax 320kg, hydrochloric acid 6kg and water 25kg, in 25 ℃～30 ℃ following continuously stirring reactions 40 hours.With this silicone resin condensation polymer solution secondary filter, add 1000kg propyl carbinol thinner, stir; Add tensio-active agent 3kg again, mix.Blowing, the sealing splendid attire is in plastic tank.
This silicone resin rigidity-increasing dope is after plated film is used curing, and the pencil hardness that records coating reaches more than the 6H; Excellent corrosion resistance.
Embodiment 4
In the 2000L enamel reaction still, adding Union carbide A-162 1200kg, silicon were latax 600kg, acetate 15kg and water 25kg, in 25 ℃～30 ℃ following continuously stirring reactions 30 hours.With this silicone resin condensation polymer solution secondary filter, add 2000kg propyl carbinol thinner, stir; Add tensio-active agent 5.5kg again, mix.Blowing, the sealing splendid attire is in plastic tank.
This silicone resin rigidity-increasing dope is after plated film is used curing, and the pencil hardness that records coating reaches more than the 6H; Excellent corrosion resistance.
Claims (7)
1. transparent organic silicon rigidity-increasing dope is meant to be applied to the silicone resin coating material that can form behind the base material with base material bonding excellence, hard and compact, transparent bright and clean coating especially.
2. the described transparent organic silicon rigidity-increasing dope of claim 1, its concrete implementing process is as follows:
Under the normal temperature, be that latax, polymerizing catalyst and water add in the reaction vessel by a certain percentage with methyl trialkoxysilane, silicon, continuously stirring reaction 10～50 hours becomes homogeneous phase up to reaction solution, and this is the silicone resin condensation polymer.This condensation polymer solution is filtered, add an amount of diluting solvent, stir, add an amount of polyether modified siloxane again, mix, so promptly make the silicone resin rigidity-increasing dope as tensio-active agent.
3. the described methyl trialkoxysilane of claim 2 mainly is meant methyltrimethoxy silane, Union carbide A-162.
4. the described silicon of claim 2 is latax, its SiO
2Content is generally 20%～40%.This silicon is the consumption of latax, generally is 10%～90% of methyl trialkoxysilane weight, and suitable consumption is 25%～75%.
5. the described polymerizing catalyst of claim 2 can be organic acid, mineral acid, metal carboxylate, acetylacetonate complex.Organic acid comprises acetate, propionic acid, butyric acid, valeric acid, maleic acid and stearic acid; Mineral acid comprises hydrochloric acid, hydrofluoric acid, nitric acid, sulfuric acid, chloric acid and hydrogen peroxide; Metal carboxylate is with formula (RCOO)
nThe compound that M represents, wherein R represents C
1～22Fat base or alicyclic radical, M are represented Ni, Ti, Pt, Rh, Co, Fe, Ru, Os, Pd, Ir and Al; N is the valency of M; This metal carboxylate can be acid anhydride or hydrate.Acetylacetonate complex is to comprise and negatively charged ion acac
-The complex compound of coordinate atoms metal.The consumption of polymerizing catalyst generally is 0.001%～10% of a methyl trialkoxysilane weight.
6. the described diluting solvent of claim 2 comprises ethanol, Virahol, propyl carbinol.Its consumption generally is 5%～200% of a prepared organic silicone resin condensation polymer weight, and suitable consumption is 25%～150%.
7. the described transparent organic silicon rigidity-increasing dope of claim 1 can carry out plated film by methods such as spraying, dip-coating, roller coat, vacuum sprayings.After matrix or substrate coated this silicone resin rigidity-increasing dope, the heating baked and cured, solidification value is 50 ℃～80 ℃ usually, 0.5～3 hour set time.The silicone resin that so makes is filmed, and its any surface finish is transparent, hard wear resistant, and pencil hardness can reach 6H～9H.
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| CNA2006100539506A CN101168645A (en) | 2006-10-25 | 2006-10-25 | Transparent organic silicon rigidity-increasing dope |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153754A (en) * | 2011-03-11 | 2011-08-17 | 深圳丹邦科技股份有限公司 | Silicone resin, latex paint thereof, preparation methods of silicone resin and latex paint thereof and coating |
| CN102260455A (en) * | 2010-05-29 | 2011-11-30 | 比亚迪股份有限公司 | A coating, and an optical element comprising the coating |
| CN101928515B (en) * | 2009-06-22 | 2012-12-12 | 比亚迪股份有限公司 | Sol and thin film material formed by same |
| CN102317391B (en) * | 2009-01-09 | 2014-10-15 | 莫门蒂夫性能材料股份有限公司 | Silane coating compositions containing silicon-based polyether copolymers, methods for coating metal surfaces and articles made therefrom |
| CN105602307A (en) * | 2016-03-02 | 2016-05-25 | 沈阳化工大学 | Waterproof transparent coating for protecting cultural relic |
-
2006
- 2006-10-25 CN CNA2006100539506A patent/CN101168645A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102317391B (en) * | 2009-01-09 | 2014-10-15 | 莫门蒂夫性能材料股份有限公司 | Silane coating compositions containing silicon-based polyether copolymers, methods for coating metal surfaces and articles made therefrom |
| CN101928515B (en) * | 2009-06-22 | 2012-12-12 | 比亚迪股份有限公司 | Sol and thin film material formed by same |
| CN102260455A (en) * | 2010-05-29 | 2011-11-30 | 比亚迪股份有限公司 | A coating, and an optical element comprising the coating |
| CN102153754A (en) * | 2011-03-11 | 2011-08-17 | 深圳丹邦科技股份有限公司 | Silicone resin, latex paint thereof, preparation methods of silicone resin and latex paint thereof and coating |
| CN102153754B (en) * | 2011-03-11 | 2013-06-26 | 深圳丹邦科技股份有限公司 | Silicone resin, latex paint thereof, preparation methods of silicone resin and latex paint thereof and coating |
| CN105602307A (en) * | 2016-03-02 | 2016-05-25 | 沈阳化工大学 | Waterproof transparent coating for protecting cultural relic |
| CN105602307B (en) * | 2016-03-02 | 2018-01-26 | 沈阳化工大学 | A kind of water-fast clear coat of historical relic's protection |
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Open date: 20080430 |