CN102181226A - Carbamate coating serving as monocomponent nonvolatile solvent and preparation method thereof - Google Patents
Carbamate coating serving as monocomponent nonvolatile solvent and preparation method thereof Download PDFInfo
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Abstract
The invention provides a carbamate coating serving as a monocomponent nonvolatile solvent and a preparation method thereof. The coating comprises toluylene diisocyanate (TDI) 20/80, polyether N-210, polyether N-330, dibutyltin dilaurate, an active diluent, a metal oxide foam inhibitor and other aids. The preparation method comprises the following steps of: dehydrating the polyether N-210 and the polyether N-330 in vacuum at the temperature of higher than 100 DEG C; transferring dehydrated polyether into another reaction kettle, adding the TDI and the active diluent and undergoing a polymerization reaction at temperature of between 85 DEG C and 95 DEG C at the vacuum degree of lower than 0.1 MPa; and after the reaction, adding the metal oxide foam inhibitor, an ultraviolet absorbent, a pigment, a filler and other aids and uniformly stirring. The coating has the advantages of nontoxicity, environmental friendliness, high adhesion, high medium resistance, smooth and bright paint film, and the like, can be painted with thick slurry in rusty state, and is a functional special coating which is accordant with the high-end technical development trend of coatings.
Description
Technical field
The present invention relates to a kind of carboxylamine ester paint and preparation method thereof, relate in particular to a kind of single component non-volatility solvent carboxylamine ester paint and preparation method thereof.
Background technology
Generally use the carboxylamine ester paint under corrosive environment, equipment being carried out rotproofing, this paint medium adaptability is strong, and antiseptic property is good, moderate cost, easy-to-use, be used widely in fields such as chemical industry, machinery, metallurgy, boats and ships, railway, harbours at present.
The carboxylamine ester paint is divided into two-pack and two kinds of forms of single component, two-pack carboxylamine ester paint is arranged in pairs or groups by the ratio of component and is regulated its performance, advantage is that this coating is stablized, easily to store, be subjected to environmental change to influence little, shortcoming is that on-the-spot amount of preparation is difficult for grasping, need the fixed mixing ratio amount, stir, coatings formulated is tood many or too much for use if make, just solidified after for some time, caused waste easily.Single component carboxylamine ester paint has preparation simply, and coating film forming is controlled, and easy to operate, time saving and energy saving advantage is the desirable coating that anticorrosive construction is carried out in many fields.
Traditional protective system contains a large amount of volatile organic solvents, its existence causes a build of coating below 50 μ m, do not reach the ideal preservative effect, obtain thicker thickness and must increase the coating number of times, not only time-consuming, and a large amount of volatile organic solvents volatilization damage with contaminate environment with to workmen's health, do not meet requirements of green environmental protection, the direction of coating industry reform and innovation is not use volatile organic solvent.Non-volatility organic solvent coating is meant the coating that does not contain volatile organic solvent or water in a broad aspect, says so narrowly to refer to not contain the liquid coating of volatile organic solvent.
Non-volatility organic solvent coating is meant and adopts the liquid coating of reactive thinner as solvent medium, reactive thinner plays solvent and softening agent, can reduce simultaneously the viscosity of coating, make coating decoration convenient, use reactive thinner and use traditional volatile organic solvent and softening agent different, in its film process, reactive thinner and resin generation crosslinking reaction, become the integral part of filming, strengthened the sticking power of film on medium.Studies show that the reactive thinner kind that can be used in carbamate type coating is more, as low molecular weight diol or polyvalent alcohol, hindered amine, aldimine, ketoimine, oxazolidine etc.Reactive thinner has the active higher group that can react with isocyanic ester, thereby is difficult to be applied to the single-component system, is generally used for preparing dual-component coating.For example Chinese patent CN200810197920 adopts and has the slight collateralization polyvalent alcohol of ester group and ether as reactive thinner, the preparation double-composition polyurethane waterproof paint, because the molecular weight of the reactive thinner that uses is lower, after isocyanate-crosslinked film forming, cause that paint film is more crisp, degradation problem under the tensile strength.
In addition in the synthetic production of carbamate, in the raw material micro-moisture have polyreaction the time implode takes place easily, in order to prevent the generation of implode, when building-up reactions, add organic solvents such as toluene, make that building-up reactions is comparatively gentle carries out, but organic solvents such as toluene can produce in producing and using and pollute to environment, and its influence will continue for some time as source of pollution, according to the standard of coating industry, should ban use of toluene; In order to prevent the generation of implode, when polyreaction, feed stable that nitrogen can keep reacting, make the production operation complexity but feed nitrogen, production cost increases.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of single component non-volatility solvent carboxylamine ester paint and preparation method thereof, this coating does not adopt volatile solvent, film forming is according to demand used in application, and the sticking power between reinforcing membrane and the medium, the solid content of material improves in the paint film.
At purpose of the present invention, in a first aspect of the present invention, the invention provides a kind of single component non-volatility solvent carboxylamine ester paint, comprising: tolylene diisocyanate (TDI) 20/80,20 ~ 30%; Polyethers N-210,15 ~ 25%; Polyethers N-330,25 ~ 35%; Dibutyl tin laurate, 0.3 ~ 1%; Reactive thinner, 4 ~ 15%; Potter's clay, 0 ~ 10%; UV light absorber, 0 ~ 1.5%; The metal oxide suds suppressor, 5 ~ 8%; Silicon-dioxide, 0 ~ 2.5%; And titanium dioxide, 0 ~ 10%; Wherein, described reactive thinner is hexamethylene diisocyanate (HDI), and described metal oxide suds suppressor is selected from a kind of in calcium oxide, magnesium oxide, the barium oxide.
At purpose of the present invention, in a second aspect of the present invention, the invention provides a kind of preparation method of single component non-volatility solvent carboxylamine ester paint, comprising:
The first step: the polyethers N-210 of polyethers N-330 and 96 ~ 98% meterings are joined in first reactor, and below vacuum tightness 0.1MPa, temperature prepared anhydrous polyethers greater than under 100 ℃ of conditions dewatering time 6-8 hour;
Second step: the anhydrous polyethers of the first step preparation is transferred in second reactor, the tolylene diisocyanate, dibutyl tin laurate, the reactive thinner that add corresponding proportioning, below vacuum tightness 0.1MPa, temperature is controlled at 85 ~ 95 ℃, polyreaction 3-4 hour, obtain performed polymer;
The 3rd step: the performed polymer that the second step polyreaction is obtained changes in the 3rd reactor, the polyethers N-210, potter's clay, UV light absorber, metal oxide suds suppressor, silicon-dioxide and the titanium dioxide that add remaining 2 ~ 4% meterings, below vacuum tightness 0.1MPa, stirred 0.5-1 hour, and treated that it was cooled to the room temperature discharging.
Single component non-volatility solvent carboxylamine ester paint provided by the invention, reactive thinner is a hexamethylene diisocyanate, under technology of the present invention, utilize aromatic isocyanate and the aliphatic isocyanates difference on reactive behavior, tolylene diisocyanate all reacts, and hexamethylene diisocyanate does not participate in or minute quantity participates in reaction, thereby plays the effect of thinner.In being coated with membrane process, because the influence of moisture in base material or the environment, reactive thinner (hexamethylene diisocyanate) can react rapidly, and the product of reaction is present in the coating, has improved the solid content of filmogen.The carbon dioxide that the metal oxide suds suppressor produces in can the absorbing coating solidification process generates carbonate and is present in the coating as the filler of coating, makes the paint film smooth, has solved the problem of bubble in coating decoration effectively.
The preparation method of single component non-volatility solvent carboxylamine ester paint provided by the invention, its production process is operated under vacuum tightness is lower than 0.1MPa, make the temperature of reaction needed reduce, in the first step dehydration, can take out water molecules and other small molecular weight material, fundamentally guarantee the existence of non-volatility solvent in the coating.
The advantage of a kind of single component non-volatility solvent carboxylamine ester paint provided by the invention is not adopt volatile solvent, film forming is according to demand used in application, and the sticking power between reinforcing membrane and the medium, can realize the thick-slurry type application, an application can reach more than 120 microns, preservative effect is better, the medium-resistance excellence.Adopt preparation method of the present invention to solve the carbonic acid gas bubble difficult problem that coating produces effectively in construction process, the paint film smooth, it is easy to use to construct, environment is not produced pollution, harmless, meet the coating industry requirements of green environmental protection, coating provided by the invention is applicable to various substrate surfaces, has great universality.
Embodiment
The following describes according to single component non-volatility solvent carboxylamine ester paint of the present invention and preparation method thereof.
At first explanation is according to single component non-volatility solvent carboxylamine ester paint of the present invention.
Single component non-volatility solvent carboxylamine ester paint of the present invention comprises (by weight percentage):
Tolylene diisocyanate (TDI) 20/80,20 ~ 30%;
Polyethers N-210,15 ~ 25%;
Polyethers N-330,25 ~ 35%;
Dibutyl tin laurate (DBTDL), 0.3 ~ 1%;
Reactive thinner, 4 ~ 15%;
Potter's clay, 0 ~ 10%;
UV light absorber, 0 ~ 1.5%;
The metal oxide suds suppressor, 5 ~ 8%;
Silicon-dioxide, 0 ~ 2.5%; And
Titanium dioxide, 0 ~ 10%.
In foundation single component non-volatility solvent carboxylamine ester paint of the present invention, polyaddition reaction takes place in polyethers N-210, polyethers N-330 and tolylene diisocyanate (TDI), forms performed polymer.Wherein, the content of tolylene diisocyanate is preferably 25%, and the content of polyethers N-210 is preferably 20%, and the content of polyethers N-330 is preferably 30%.
In foundation single component non-volatility solvent carboxylamine ester paint of the present invention, reactive thinner is hexamethylene diisocyanate (HDI), and content is preferably 12.5%.Under synthesis technique of the present invention, utilize aromatic isocyanate and the aliphatic isocyanates difference on reactive behavior, tolylene diisocyanate all reacts, and hexamethylene diisocyanate does not participate in or minute quantity participates in reaction, reduce the viscosity of system, thereby played the effect of thinner.In being coated with membrane process, because the influence of moisture in base material or the environment, reactive thinner (hexamethylene diisocyanate) can react rapidly, and the product of reaction is present in the coating, improve the solid content of filmogen, thoroughly avoided the use of volatile organic solvent.
According in the single component non-volatility solvent carboxylamine ester paint of the present invention, described metal oxide suds suppressor is selected from a kind of in calcium oxide, magnesium oxide, the barium oxide.The preferred calcium oxide that adopts.When adopting calcium oxide, the calcium hydroxide that calcium oxide and water generate absorbs isocyanic ester and water reacts the carbonic acid gas that produces, and forms precipitation of calcium carbonate and be stored in the coating as filler, thereby solve the problem that chemistry steeps.
Secondly, the preparation method of foundation single component non-volatility solvent carboxylamine ester paint of the present invention is described.
Preparation method according to single component non-volatility solvent carboxylamine ester paint of the present invention comprises step:
The first step: the polyethers N-210 of polyethers N-330 and 96 ~ 98% meterings is joined in first reactor, and below vacuum tightness 0.1MPa, temperature prepares anhydrous polyethers greater than dehydration under 100 ℃ of conditions 6-8 hour;
Second step: the anhydrous polyethers of the first step preparation is transferred in second reactor, the tolylene diisocyanate, dibutyl tin laurate, the reactive thinner that add corresponding proportioning, vacuum tightness is below 0.1MPa in this reactor, temperature is controlled at 85 ~ 95 ℃, polyreaction 3-4 hour, obtain performed polymer;
The 3rd step: the performed polymer of the second step gained is transferred in the 3rd reactor, the polyethers N-210, potter's clay, UV light absorber, metal oxide-type suds suppressor, silicon-dioxide and the titanium dioxide that add remaining 2 ~ 4% meterings, control vacuum tightness is below 0.1MPa, stirred 0.5-1 hour, and treated that it was cooled to the room temperature discharging.
In the foundation preparation method of single component non-volatility solvent carboxylamine ester paint of the present invention, institute all carries out under vacuum state in steps, and vacuum tightness is preferably 0.06 ~ 0.1MPa.Owing to adopt whole process under vacuum tightness is lower than 0.1MPa, to operate in the production technique, make the temperature of reaction needed reduce, in the first step dehydration, can take out water molecules and other small molecular weight material simultaneously, fundamentally guaranteed the existence of non-volatility solvent.
In the foundation preparation method of single component non-volatility solvent carboxylamine ester paint of the present invention, in the described the first step, dehydration temperaturre is preferably 105 ~ 120 ℃, and dewatering time is preferably 6 ~ 8 hours.
In the foundation preparation method of single component non-volatility solvent carboxylamine ester paint of the present invention, in described second step, polymeric reaction temperature is preferably 90 ℃, and polymerization reaction time is preferably 3 ~ 4 hours.Under this temperature and vacuum tightness, tolylene diisocyanate can react, but hexamethylene diisocyanate does not participate in or minute quantity participates in reaction.
Single component non-volatility solvent carboxylamine ester paint of the present invention can be realized the thick-slurry type application, and an application can reach more than 120 microns, belongs to low and requires surface treatment paint, has saved resource and time; Based on its excellent sticking power,, has great universality applicable to various substrate surfaces; Belong to a kind of functional type speciality coating that meets coating high-end technology development trend.
The existing relatively protective system commonly used of single component non-volatility solvent carboxylamine ester paint of the present invention has been compared following advantage:
(1) substrate surface treatment S t2 level can be simplified complicated pretreatment procedure, simplifies loaded down with trivial details supporting multiple tracks coating process and significantly improves work efficiency, reduction expense;
(2) can be with rust, be with the bonding force of old paint film application and various paint films good;
(3) construction temperature 15-40 ℃, no greasy weather, humidity, dew-point temperature restriction, once the construction build of filming can reach 100-150 μ m, can reduce a large amount of artificial relatively;
(4) product does not contain various You Ji Suan ﹑ mineral acids, the antirust color stuffings of toxic heavy metal such as not leaded, chromium, and the nontoxic level in the true border of paint film, in process of production, all raw material and auxiliary agent all are converted into finished product, the non-volatility solvent discharge.
(5) solvent free is saved the volatile solvent consumption in a large number, avoids the wasting of resources and reliable in quality, but long-effective corrosion can reduce the huge resource, the energy consumption that are caused because of the volatile solvent use.
Provide the embodiment of several single-component non-volatility solvent carboxylamine ester paints of the present invention below; embodiment is for technical scheme of the present invention is described better; do not limit the scope of the invention; make without departing from the inventive concept of the premise and somely be equal to alternatively, all should be considered as belonging to the protection domain that claims of the present invention are determined.。
Embodiment 1
By percentage to the quality, component and content are: tolylene diisocyanate (TDI) 20/80,20%; Polyethers N-210,15%; Polyethers N-330,25%; Dibutyl tin laurate, 0.3%; Hexamethylene diisocyanate, 15%; Potter's clay, 10%; UV light absorber, 1.5%; Magnesium oxide, 8%; Silicon-dioxide, 2.5%; Titanium dioxide, 2.7%.
Preparation technology is: the first step: the polyethers N-210 of polyethers N-330 and 96% metering is added in first reactor, and pump vacuumizes, and treats that vacuum tightness is 0.1MPa, is warming up to 105 ℃ of dehydrations, and insulation dehydration 8 hours obtains anhydrous polyethers; Second step: the anhydrous polyethers of the first step preparation is transferred in second reactor, vacuum tightness is 0.07MPa in the tolylene diisocyanate and the reactive thinner (hexamethylene diisocyanate) that add corresponding proportioning, this reactor, and temperature is controlled at 85 ℃, polyreaction 3 hours obtains performed polymer; The 3rd step: the second step gained performed polymer is changed in the 3rd reactor, the polyethers N-210, potter's clay, UV light absorber, magnesium oxide, silicon-dioxide and the titanium dioxide that add remaining 4% metering, control vacuum tightness 0.06MPa stirred 1 hour, treated that it is cooled to the room temperature discharging.
Embodiment 2
By percentage to the quality, component and content are: tolylene diisocyanate (TDI) 20/80,30%; Polyethers N-210,25%; Polyethers N-330,35%; Dibutyl tin laurate, 1%; Hexamethylene diisocyanate, 4%; Barium oxide, 5%.
Preparation technology is: the first step: the polyethers N-210 of polyethers N-330 and 98% metering is added in first reactor, and pump vacuumizes, and treats that vacuum tightness is 0.06MPa, is warming up to 110 ℃ of dehydrations, and the insulation dehydration obtained anhydrous polyethers in 6 hours; Second step: the anhydrous polyethers of the first step preparation is transferred in second reactor, vacuum tightness is 0.07MPa in the tolylene diisocyanate and the reactive thinner (hexamethylene diisocyanate) that add corresponding proportioning, this reactor, and temperature is controlled at 95 ℃, polyreaction 3 hours obtains performed polymer; The 3rd step: the second step gained performed polymer is changed in the 3rd reactor, add polyethers N-210, the barium oxide of remaining 2% metering, control vacuum tightness 0.08MPa stirred 0.8 hour, treated that it is cooled to the room temperature discharging.
Embodiment 3
By percentage to the quality, component and content are: tolylene diisocyanate (TDI) 20/80,22%; Polyethers N-210,15%; Polyethers N-330,30%; Dibutyl tin laurate, 0.5%; Hexamethylene diisocyanate, 12.5%; UV light absorber, 1.5%; Calcium oxide, 6%; Silicon-dioxide, 2.5%; Titanium dioxide, 10%.
Preparation technology is: the first step: the polyethers N-210 of polyethers N-330 and 97% metering is added in first reactor, and pump vacuumizes, and treats that vacuum tightness is 0.1MPa, is warming up to 120 ℃ of dehydrations, and insulation dehydration 8 hours obtains anhydrous polyethers; Second step: the anhydrous polyethers of the first step preparation is transferred in second reactor, vacuum tightness is 0.07MPa in the tolylene diisocyanate and the reactive thinner (hexamethylene diisocyanate) that add corresponding proportioning, this reactor, and temperature is controlled at 90 ℃, polyreaction 4 hours obtains performed polymer; The 3rd step: the performed polymer of the second step gained is changed in the 3rd reactor, the polyethers N-210, UV light absorber, calcium oxide, silicon-dioxide and the titanium dioxide that add remaining 3% metering, control vacuum tightness 0.1MPa stirred 0.6 hour, treated that it is cooled to the room temperature discharging.
The performance test results of embodiment 1-3 sees Table 1.
Table 1
| Performance | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Sticking power (drawing back method, carbon steel/carbon steel) | 7.16MPa | 6.08MPa | 7.85 MPa |
| Salt fog resistance | 1600h | 1500h | 2000h |
| Ultraviolet aging resistance | 1000h | 800h | 1000 h |
| Solid content | 97% | 98% | 99% |
| Resistance to medium | 100 days | 90 days | 100 days |
| Set time | 15h | 11h | 8h |
By table 1 as seen, single component non-volatility solvent carboxylamine ester paint of the present invention, its sticking power, salt fog resistance, ultraviolet aging resistance, solid content, antiseptic property, resistance to medium, set time, these aspects were all more excellent, proved absolutely the superiority of single component non-volatility solvent carboxylamine ester paint of the present invention, suitable to the thick slurry application of band rust, belong to a kind of functional type speciality coating that meets coating high-end technology development trend.
Claims (7)
1. single component non-volatility solvent carboxylamine ester paint comprises:
Tolylene diisocyanate (TDI) 20,/80 20 ~ 30%;
Polyethers N-210 15 ~ 25%;
Polyethers N-330 25 ~ 35%;
Dibutyl tin laurate 0.3 ~ 1%;
Reactive thinner 4 ~ 15%;
Potter's clay 0 ~ 10%;
UV light absorber 0 ~ 1.5%;
Metal oxide suds suppressor 5 ~ 8%;
Silicon-dioxide 0 ~ 2.5%;
Titanium dioxide 0 ~ 10%;
Single component non-volatility solvent carboxylamine ester paint according to claim 1 is characterized in that described reactive thinner is a hexamethylene diisocyanate, and its content is preferably 12.5%.
2. single component non-volatility solvent carboxylamine ester paint according to claim 1 and 2 is characterized in that, described metal oxide suds suppressor is selected from a kind of in calcium oxide, magnesium oxide, the barium oxide.
3. the preparation method of a single component non-volatility solvent carboxylamine ester paint is used for preparation according to each described single component non-volatility solvent carboxylamine ester paint of claim 1 ~ 3, comprises step:
The first step: the polyethers N-210 of polyethers N-330 and 96 ~ 98% meterings is joined in first reactor, and below vacuum tightness 0.1MPa, temperature prepares anhydrous polyethers greater than dewatering under 100 ℃ of conditions;
Second step: the anhydrous polyethers of the first step preparation is transferred in second reactor, the tolylene diisocyanate, dibutyl tin laurate, the reactive thinner that add corresponding proportioning, below vacuum tightness 0.1MPa, temperature is controlled at 85 ~ 95 ℃, carry out polyreaction, the preparation performed polymer;
The 3rd step: the performed polymer of second step preparation is changed in the 3rd reactor, the polyethers N-210, potter's clay, UV light absorber, metal oxide suds suppressor, silicon-dioxide and the titanium dioxide that add remaining 2 ~ 4% meterings, below vacuum tightness 0.1MPa, stir, treat that it is cooled to the room temperature discharging.
4. according to the preparation method of the described single component non-volatility of claim 4 solvent carboxylamine ester paint, it is characterized in that dehydration, polymerization, be stirred under the vacuum state and carry out, vacuum tightness is 0.06 ~ 0.1Mpa.
5. according to the preparation method of the described single component non-volatility of claim 4 solvent carboxylamine ester paint, it is characterized in that dehydration temperaturre is preferably 105 ~ 120 ℃, dewatering time is preferably 6 ~ 8 hours.
6. according to the preparation method of the described single component non-volatility of claim 4 solvent carboxylamine ester paint, it is characterized in that polymeric reaction temperature is preferably 90 ℃, the reaction times is preferably 3 ~ 4 hours.
7. according to the preparation method of the described single component non-volatility of claim 4 solvent carboxylamine ester paint, it is characterized in that, churning time be 0.6-1 hour (also can write 0.5-1 hour herein, will revise embodiment 3 so, could? please decide).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102876219A (en) * | 2012-09-26 | 2013-01-16 | 苏州汾湖电梯有限公司 | Anti-rust coating for elevator panel |
| CN103952070A (en) * | 2014-04-17 | 2014-07-30 | 葫芦岛亿拓实业有限公司 | Solvent-free polymerized anticorrosive coating and preparation method thereof |
| CN105061347A (en) * | 2015-07-29 | 2015-11-18 | 北京东方雨虹防水技术股份有限公司 | Novel oxazolidine, preparation method, application, and mono-component polyurethane waterproof paint |
| CN111040611A (en) * | 2019-12-19 | 2020-04-21 | 湖南太子化工涂料有限公司 | Antirust coating suitable for engineering machinery and preparation method thereof |
| CN113372804A (en) * | 2021-05-27 | 2021-09-10 | 锦绣防水科技有限公司 | Single-component polyurethane waterproof paint capable of forming film once and preparation method thereof |
| CN114015345A (en) * | 2021-11-04 | 2022-02-08 | 上海三棵树防水技术有限公司 | Anti-sagging polyurethane waterproof coating of water curing system and preparation method thereof |
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2011
- 2011-03-22 CN CN2011100705808A patent/CN102181226A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102876219A (en) * | 2012-09-26 | 2013-01-16 | 苏州汾湖电梯有限公司 | Anti-rust coating for elevator panel |
| CN103952070A (en) * | 2014-04-17 | 2014-07-30 | 葫芦岛亿拓实业有限公司 | Solvent-free polymerized anticorrosive coating and preparation method thereof |
| CN105061347A (en) * | 2015-07-29 | 2015-11-18 | 北京东方雨虹防水技术股份有限公司 | Novel oxazolidine, preparation method, application, and mono-component polyurethane waterproof paint |
| CN111040611A (en) * | 2019-12-19 | 2020-04-21 | 湖南太子化工涂料有限公司 | Antirust coating suitable for engineering machinery and preparation method thereof |
| CN113372804A (en) * | 2021-05-27 | 2021-09-10 | 锦绣防水科技有限公司 | Single-component polyurethane waterproof paint capable of forming film once and preparation method thereof |
| CN114015345A (en) * | 2021-11-04 | 2022-02-08 | 上海三棵树防水技术有限公司 | Anti-sagging polyurethane waterproof coating of water curing system and preparation method thereof |
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Application publication date: 20110914 |