CN103937388B - Nano combined gel coat of weather resistant and preparation method thereof - Google Patents
Nano combined gel coat of weather resistant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses the nano combined gel coat of a kind of weather resistant, it is grouped into by the one-tenth of following weight part: unsaturated polyester resin 100 parts, vinylbenzene 10-30 part, modified nano-ZnO 10-25 part, talcum powder 5-8 part, titanium dioxide 3-5 part, thixotropic agent 1-3 part, thixotroping stablizer 0.1-0.2 part, surface modifier 0.4-1 part, mill base 0-10 part, promotor 0.1-0.4 part.The present invention also provides the preparation method of the nano combined gel coat of above-mentioned weather resistant simultaneously, comprises the following steps: 1), in unsaturated polyester resin successively add talcum powder, titanium dioxide, thixotroping stablizer and thixotropic agent; 2), in vinylbenzene add modified nano-ZnO, after high speed dispersion, join step 1) in gains; 3), to step 2) gains in add mill base, surface modifier and promotor.The nano combined gel coat of this weather resistant is mainly used in cooling tower glass fiber reinforced plastic surface.
Description
Technical field
This invention relates to nano combined gel coat of a kind of weather resistant and preparation method thereof, and the nano combined gel coat of this weather resistant is mainly used in cooling tower glass fiber reinforced plastic surface.
Background technology
Cooling tower is equipment conventional in industrial circulating water, is usually used in Steel Plant, printing and dyeing mill, Medicine Factory, nuclear power plant, air-conditioning, freezer and the field such as chemical fibre, oil.Cooling tower tower body conventional is at present generally glass reinforced plastic, and for improving the material of glass reinforced plastic visual appearance and protective glass steel structural layer not by extraneous dielectric corrosion, glass fiber reinforced plastic surface of being everlasting applies one deck gel coat.Gel coat is the kind of a kind of special applications in unsaturated polyester resin, its main constituent is macromolecular material, therefore be often exposed to when it in various environment such as sunlight, wind and rain, high temperature, severe cold, As time goes on, its weathering resistance can decline, thus causes the phenomenon such as efflorescence, variable color.For improving gel coat weather resistance, one method uses the better unsaturated polyester resin of weather resistance, another kind method is carried out preferably to the filler in gel coat, because filler can improve the physical strength of gel coat, wear-resisting, water-fast and weather resistance (Cao Xin, the research of weather resistant fire retardant glue coating resin, fibre composite, 2005,1:10-11; Zhang Huijuan, each component of gel coat on the impact of gel coat aging resistance, East China University of Science, Engineering Master paper in 2011).
Nano-ZnO is a kind of polyfunctional new oxide, and it has surface effects, volume effect, quantum size effect and macroscopical tunnel effect and the feature such as high-clarity, polymolecularity that macro object do not have.In addition, nano-ZnO also has and covers ultraviolet performance preferably, and its UV-preventing rate is up to 98%.But when filler uses, also be there is following two problems in nano-ZnO at present:
1), nano-ZnO surface energy is high, easily reunites, bad with matrix resin consistency, for addressing this problem, normal coupling agent or the tensio-active agent of using carries out surface modification to nano-ZnO at present, but this method of modifying can use a large amount of organic solvent usually, as ethanol, toluene etc., their contaminate environment, poisonous to human body, also can increase and reclaim or destroy cost (Shi Zhen etc., the Research on Surface Modification of nano-ZnO, Shanghai coating, 2008,46 (5) 1-3; Wu Wenming, Pan Lei etc., the surface modification of nano-ZnO and the preparation of ZnO/UPR matrix material, thermosetting resin, 2009,24 (5): 44).
2) its addition in matrix resin of modified at present nanoparticle is little, otherwise opposite effect can be played to the performance of resin, as reduced mechanical property, increasing that dope viscosity causes can not shaping (Wu Wenming such as grade, Pan Lei etc., the surface modification of nano-ZnO and the preparation of ZnO/UPR matrix material, thermosetting resin, 2009,24 (5): 44; Wang Haifeng, Xu Yi etc., nanometer Al
2o
3the preparation and property research of Filled PTEF matrix material, plastics industry, 2012,40 (6): 88; BauerF, etal.Preparationofsctrachandabrasionresistantpolymericna nocompositesbymonoergraftingontonanoparticles, effectoffillerpartilcesandgraftingagents, Macromol.Mater.Eng.2002,287,546-552.).Such problem also appears in the gel coat after ZnO Modified, therefore in gel coat, the addition of nano-ZnO can not be too many, otherwise gel coat viscosity can be caused to increase (thickening power), but also remarkable enhancement is not had to the weather resistance of gel coat like this.
Summary of the invention
The technical problem to be solved in the present invention is to provide nano combined gel coat of a kind of weather resistant and preparation method thereof; The nano combined gel coat of this weather resistant is mainly used in cooling tower glass fiber reinforced plastic surface.
In order to solve the problems of the technologies described above, the invention provides the nano combined gel coat of a kind of weather resistant, be grouped into by the one-tenth of following weight part: unsaturated polyester resin 100 parts, vinylbenzene 10-30 part, modified nano-ZnO 10-25 part, talcum powder 5-8 part, titanium dioxide 3-5 part, thixotropic agent 1-3 part, thixotroping stablizer 0.1-0.2 part, surface modifier 0.4-1 part, mill base 0-10 part, promotor 0.1-0.4 part.
Improvement as the nano combined gel coat of weather resistant of the present invention: the preparation method of modified nano-ZnO is:
The nano-ZnO being 10 ~ 60nm by 1 part of particle diameter is added in the deionized water of 1.5 ~ 2.5 parts (being preferably 2 parts), high-speed stirring is after 10 ~ 30 minutes, add 0.2 ~ 0.5 part of properties-correcting agent again, then pH is regulated to be 3 ~ 5 (being such as 4), be warming up to 50 ~ 70 DEG C again, insulation (50 ~ 70 DEG C) stirring reaction 1 ~ 3 hour, filters, gained filter cake under room temperature environment vacuum-drying to constant weight; Obtain modified nano-ZnO;
Described properties-correcting agent is γ-methacryloxypropyl trimethoxy silane or vinyltriethoxysilane;
Above-mentioned part is weight part.
Remarks illustrate: regulate pH to adopt usual manner to carry out, such as, 10% (weight ratio) HCl solution can be adopted to regulate.
γ-methacryloxypropyl trimethoxy silane is γ-(methacryloxypropyl) propyl trimethoxy silicane.
Further improvement as the nano combined gel coat of weather resistant of the present invention:
Described unsaturated polyester resin is adjacent benzene-neopentyl glycol type unsaturated polyester resin, isophthalic-neopentyl glycol type unsaturated polyester resin;
Thixotropic agent is gas phase SiO
2, specific surface area is 150 ~ 380m
2/ g;
Thixotroping stablizer is the PR600 type thixotroping stablizer that Ke Laien (Clariant) company produces;
Surface modifier is any three kinds or four kinds in BYK-A515, BYK-A555, BYK-S706 and JS-V966;
Mill base is azo pigment class, color lake class, copper phthalocyanine class, condensed ring class and organic macromolecule pigment;
Promotor is cobalt iso-octoate.
The present invention also provides the preparation method of the nano combined gel coat of above-mentioned weather resistant simultaneously, comprises the steps:
1), first unsaturated polyester resin is put into Scattered Kettle, stir lower priority and add talcum powder, titanium dioxide, thixotroping stablizer and thixotropic agent, be uniformly dispersed;
2), in vinylbenzene add modified nano-ZnO, after high speed dispersion, join step 1) in the mixture that formed; Homogeneous phase mixing;
3), to step 2) gains in add mill base, surface modifier and promotor, after uniform stirring, obtain the nano combined gel coat of weather resistant.
In the present invention, room temperature refers to 15 ~ 25 DEG C; High-speed stirring is the rotating speed of 1000-2000rpm; All the other stirrings are the rotating speed of 500 ~ 800rpm.
In view of the technological deficiency existing for above-mentioned prior art, the present invention is the nano combined gel coat of a kind of weather resistant of exploitation, and the modified nano-ZnO of use is carried out modification as a kind of filler to gel coat.The preparation method of modified nano-ZnO of the present invention (namely, nano-ZnO is carried out to the method for surface modification) take water as solvent, pollution-free, little to human injury, properties-correcting agent is the silane coupling agent with double bond simultaneously, its can with unsaturated polyester resin generation copolyreaction, therefore can bonding force between reinforcing filler and matrix, nano-ZnO can be reduced and gel coat mechanical property is produced destroy.In addition, above-mentioned method of modifying set by the present invention can carry out good modification to nano-ZnO, therefore its adding proportion in gel coat is higher, the viscosity of gel coat can not be increased, therefore it can significantly improve the weather resistance of gel coat on the one hand, also can strengthen on the other hand the performances such as wear-resisting, the hardness of gel coat, thus reduce the interpolation of other hard filler.
In sum, the present invention is directed to existing cooling tower glass fiber reinforced plastic surface gel coat weather resistance bad, easy efflorescence, this present situation easy to change, by adding the modified nano-ZnO with good ultraviolet line function of shielding in gel coat, prepared the nano combined gel coat of weather resistant.
The nano combined gel coat of weather resistant prepared by the present invention adopts the artificially-aged method of acceleration of the current international practice and uses standard convention to carry out experimental evaluation with reference to U.S. ASTM-G154 non-metallic material ultraviolet fluorescence equipment, the artificial accelerated aging time is 1000 hours, then full-automatic color difference meter (SC-80C is used, Beijing Kang Guang opticinstrument company limited) characterize colourimetric number change (△ E) of aging front and back coating and yellow value degree changes (△ Yid), and the coating that detects by an unaided eye is with or without efflorescence.Experimental result shows, the nano combined gel coat artificial accelerated aging of weather resistant of the present invention is after 1000 hours, and its △ E≤1.5, △ Yid≤1.5, coatingsurface is without efflorescence.
Embodiment
Embodiment 1,
1), the surface modification (that is, the preparation method of modified nano-ZnO) of nano-ZnO:
Taking 100g nano-ZnO (particle diameter 20nm) is added in 200g deionized water, high-speed stirring adds the γ-methacryloxypropyl trimethoxy silane of 20g after 10 minutes, and use 10% (weight ratio) HCl regulation system pH to be 4, be warming up to 50 DEG C subsequently, and keep this temperature stirring reaction 3 hours, filter, gained filter cake in vacuum-drying under room temperature environment to constant weight; Obtain modified nano-ZnO.
2), the preparation of the nano combined gel coat of weather resistant
(1), by adjacent benzene-neopentyl glycol type unsaturated polyester resin 100 parts adds in Scattered Kettle, talcum powder 8 parts under stirring, is added, titanium dioxide 5 parts, thixotropic agent--gas phase SiO
2(specific surface area 150m
2/ g) 3 parts, thixotroping stablizer---PR6000.2 part; Stir 30 minutes; Thus realize being uniformly dispersed.
(2), join in 10 parts of vinylbenzene by modified nano-ZnO 10 parts, high speed dispersion joins in the mixture that step (1) formed after 30 minutes, uniform stirring 0.5 hour; Thus realize Homogeneous phase mixing;
(3) mill base 0 part, surface modifier 0.5 part (being obtained by mixing according to the weight ratio of 1:1:1 by BYK-A515, BYK-A555, BYK-S706) and promotor---cobalt iso-octoate 0.1 part is added in the mixture, formed to step (2), uniform stirring, after 0.5 hour, obtains the nano combined gel coat of weather resistant.
Comparative example 1-1,
By embodiment 1 step 1) in " adding the γ-methacryloxypropyl trimethoxy silane of 20g " make into " adding the γ-methacryloxypropyl trimethoxy silane of 15g ", the other the same as in Example 1.
Comparative example 1-2,
By embodiment 1 step 1) in " adding 20g γ-methacryloxypropyl trimethoxy silane " make into " adding 60g γ-methacryloxypropyl trimethoxy silane ", the other the same as in Example 1.
Comparative example 1-3,
By embodiment 1 step 1) in " adding 20g γ-methacryloxypropyl trimethoxy silane " make into " adding 20g3-aminopropyltriethoxywerene werene ", the other the same as in Example 1.
Comparative example 1-4,
In embodiment 1, " add 20g γ-methacryloxypropyl trimethoxy silane " make into " adding 20g γ-glycidyl ether oxygen propyl trimethoxy silicane ", the other the same as in Example 1.
Comparative example 1-5,
By embodiment 1 step 1) in reaction be modified to " 40 DEG C stirring reaction 4 hours " by " 50 DEG C stirring reaction 3 hours "; The other the same as in Example 1.
Comparative example 1-6,
By embodiment 1 step 1) in reaction be modified to " 80 DEG C stirring reaction 3 hours " by " 50 DEG C stirring reaction 3 hours "; The other the same as in Example 1.
Comparative example 1-7,
Through embodiment 1 step 2) in the consumption of modified nano-ZnO make 8 parts into by 10 parts; The other the same as in Example 1.
After nano combined gel coat film-forming above-described embodiment 1 and comparative example 1-1 ~ 1-7 prepared, artificial accelerated aging 1000h, its performance is in table 1 (detection method as described above).
Table 1
△E | △Yid | With or without efflorescence | |
Embodiment 1 | 1.5 | 1.5 | Nothing |
Comparative example 1-1 | 1.7 | 2.0 | Have |
Comparative example 1-2 | 1.8 | 1.9 | Nothing |
Comparative example 1-3 | 2.8 | 2.9 | Have |
Comparative example 1-4 | 2.5 | 2.6 | Have |
Comparative example 1-5 | 2.1 | 2.0 | Nothing |
Comparative example 1-6 | 2.0 | 2.2 | Have |
Comparative example 1-7 | 1.6 | 2.0 | Nothing |
Embodiment 2,
1), the surface modification of nano-ZnO
Taking 100g nano-ZnO (particle diameter 40nm) is added in 200g deionized water, high-speed stirring adds the γ-methacryloxypropyl trimethoxy silane of 50g after 20 minutes, and use 10% (weight ratio) HCl regulation system pH to be 4, be warming up to 70 DEG C subsequently, and keep this temperature stirring reaction 1 hour, filter, gained filter cake under room temperature environment vacuum-drying to constant weight; Obtain modified nano-ZnO.
2), the preparation of the nano combined gel coat of weather resistant
(1), by isophthalic-neopentyl glycol type unsaturated polyester resin 100 parts adds in Scattered Kettle, talcum powder 6 parts under stirring, is added, titanium dioxide 4 parts, thixotropic agent---gas phase SiO
2(specific surface area 380m
2/ g) 2 parts, thixotroping stablizer----PR6000.1 part; Stir 30 minutes, thus realize being uniformly dispersed;
(2), join in 15 parts of vinylbenzene by modified nano-ZnO 15 parts, high speed dispersion joins in the mixture that step (1) formed after 30 minutes, uniform stirring 0.5 hour; Thus realize Homogeneous phase mixing;
(3)---azo pigment 5 parts, surface modifier 1 part (being obtained by mixing according to the mass ratio of 1:1:1 by BYK-A515, BYK-A555, BYK-S706) and promotor---cobalt iso-octoate 0.1 part that adds mill base in the mixture, formed to step (2), uniform stirring, after 0.5 hour, obtains the nano combined gel coat of weather resistant.
Comparative example 2-1,
By embodiment 2 step 2) in the consumption of " modified nano-ZnO " make 0 part into by 15 parts, that is, cancel the use of " modified nano-ZnO "; All the other are with embodiment 2.
Comparative example 2-2,
By embodiment 2 step 2) in the consumption of " modified nano-ZnO " make 3 parts into by 15 parts, all the other are with embodiment 2.
Comparative example 2-3,
By embodiment 2 step 2) in the consumption of " modified nano-ZnO " make 30 parts into by 15 parts, all the other are with embodiment 2.
After nano combined gel coat film-forming embodiment 2 and comparative example 2-1 ~ 2-3 prepared, artificial accelerated aging 1000h, its performance is in table 2.
Table 2
△E | △Yid | With or without efflorescence | |
Embodiment 2 | 1.2 | 1.4 | Nothing |
Comparative example 2-1 | 3.7 | 3.8 | Have |
Comparative example 2-2 | 1.8 | 2.4 | Nothing |
Comparative example 2-3 | 1.2 | 1.4 | Nothing |
Embodiment 3.
1), the surface modification of nano-ZnO:
Take 100g nano-ZnO (particle diameter 60nm) in 200g deionized water, high-speed stirring added 50g vinyltriethoxysilane after 20 minutes, and use 10% (weight ratio) HCl regulation system pH to be 4, be warming up to 50 DEG C subsequently, and keep this temperature stirring reaction 2 hours, filter, gained filter cake under room temperature environment vacuum-drying to constant weight; Obtain modified nano-ZnO.
2), the preparation of the nano combined gel coat of weather resistant
(1), by isophthalic-neopentyl glycol type unsaturated polyester resin 100 parts adds in Scattered Kettle, talcum powder 5 parts under stirring, is added, titanium dioxide 3 parts, thixotropic agent---gas phase SiO
2(specific surface area 250m
2/ g) 1 part, thixotroping stablizer---PR6000.2 part; Churning time 30 minutes, thus realize being uniformly dispersed;
(2), join in 25 parts of vinylbenzene by modified nano-ZnO 25 parts, high speed dispersion joins in the mixture that step (1) formed after 30 minutes, uniform stirring 0.5 hour; Thus realize Homogeneous phase mixing;
(3)---copper phthalocyanine class pigment 1 part, surface modifier 0.5 part (being obtained by mixing by weight ratios such as BYK-A515, BYK-A555, BYK-S706, JS-V966) and promotor---cobalt iso-octoate 0.4 part that adds mill base in the mixture, formed to step (2), uniform stirring, after 0.5 hour, obtains the nano combined gel coat of weather resistant.
Comparative example 3-1,
By embodiment 3 step 1) in the consumption of vinyltriethoxysilane make 60g into by 50g; The other the same as in Example 3.
Comparative example 3-2,
By embodiment 3 step 1) in the consumption of vinyltriethoxysilane make 15g into by 50g; The other the same as in Example 3.
Comparative example 3-3,
By embodiment 3 step 2) in the consumption of modified nano-ZnO make 8 parts into by 25 parts; The other the same as in Example 3.
Comparative example 3-4,
Cancel the step 2 of embodiment 3) (2), that is, step (3) is made into:
(2) modified nano-ZnO 25 parts and 25 parts of vinylbenzene are first added in the mixture, formed to step (1);---copper phthalocyanine class pigment 1 part, surface modifier 0.5 part (being obtained by mixing by weight ratios such as BYK-A515, BYK-A555, BYK-S706, JS-V966) and promotor---cobalt iso-octoate 0.4 part that adds mill base again, uniform stirring, after 0.5 hour, obtains the nano combined gel coat of weather resistant.
After nano combined gel coat film-forming prepared by embodiment 3 and comparative example 3-1 ~ 3-4, artificial accelerated aging 1000h, its performance is in table 3.
Table 3
△E | △Yid | With or without efflorescence | |
Embodiment 3 | 1.1 | 1.2 | Nothing |
Comparative example 3-1 | 1.7 | 1.4 | Nothing |
Comparative example 3-2 | 1.9 | 2.0 | Nothing |
Comparative example 3-3 | 2.2 | 2.4 | Have |
Comparative example 3-4 | 2.8 | 2.9 | Have |
Found by above-described embodiment and comparative example, the nano combined gel coat of weather resistant prepared by the present invention has better weather resistance, therefore can use at cooling tower glass fiber reinforced plastic surface.
Finally, what more than enumerate is only several specific embodiments of the present invention, obviously, the invention is not restricted to above embodiment, can also have many distortion.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.
Claims (3)
1. the nano combined gel coat of weather resistant, it is characterized in that being grouped into by the one-tenth of following weight part: unsaturated polyester resin 100 parts, vinylbenzene 10-30 part, modified nano-ZnO 10-25 part, talcum powder 5-8 part, titanium dioxide 3-5 part, thixotropic agent 1-3 part, thixotroping stablizer 0.1-0.2 part, surface modifier 0.4-1 part, mill base 0-10 part, promotor 0.1-0.4 part;
The preparation method of modified nano-ZnO is:
The nano-ZnO being 10 ~ 60nm by 1 part of particle diameter is added in the deionized water of 1.5 ~ 2.5 parts, high-speed stirring is after 10 ~ 30 minutes, add 0.2 ~ 0.5 part of properties-correcting agent again, then pH is regulated to be 3 ~ 5, be warming up to 50 ~ 70 DEG C again, insulated and stirred reaction 1 ~ 3 hour, filter, gained filter cake under room temperature environment vacuum-drying to constant weight; Obtain modified nano-ZnO;
Described properties-correcting agent is γ-methacryloxypropyl trimethoxy silane or vinyltriethoxysilane;
Above-mentioned part is weight part.
2. the nano combined gel coat of weather resistant according to claim 1, is characterized in that:
Described unsaturated polyester resin is adjacent benzene-neopentyl glycol type unsaturated polyester resin, isophthalic-neopentyl glycol type unsaturated polyester resin;
Thixotropic agent is gas phase SiO
2, specific surface area is 150 ~ 380m
2/ g;
Thixotroping stablizer is PR600 type thixotroping stablizer;
Surface modifier is any three kinds or four kinds in BYK-A515, BYK-A555, BYK-S706 and JS-V966;
Mill base is azo pigment class, color lake class, copper phthalocyanine class or condensed ring class;
Promotor is cobalt iso-octoate.
3. the preparation method of the nano combined gel coat of weather resistant as claimed in claim 1 or 2, is characterized in that comprising the steps:
1), first unsaturated polyester resin is put into Scattered Kettle, stir lower priority and add talcum powder, titanium dioxide, thixotroping stablizer and thixotropic agent, be uniformly dispersed;
2), in vinylbenzene add modified nano-ZnO, after high speed dispersion, join step 1) in the mixture that formed; Homogeneous phase mixing;
3), to step 2) gains in add mill base, surface modifier and promotor, after uniform stirring, obtain the nano combined gel coat of weather resistant.
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CN105400388A (en) * | 2015-12-18 | 2016-03-16 | 福建梭罗复合材料研究有限公司 | Colorful gel coat and preparation method thereof |
CN105440897B (en) * | 2015-12-19 | 2018-08-21 | 福建梭罗复合材料研究有限公司 | A kind of piano fire-retardant black gel coat and preparation method |
CN106881881B (en) * | 2017-03-29 | 2019-06-07 | 重庆海庆新材料有限公司 | Weather-proof glass fiber reinforced plastics product vacuum imports processing method |
CN109321102A (en) * | 2018-10-11 | 2019-02-12 | 上海众挚化工科技有限公司 | A kind of gel coat and its preparation method and application for epoxy resin composite material surface |
CN110724446A (en) * | 2019-11-26 | 2020-01-24 | 常熟市建安玻璃钢制品有限公司 | Glass fiber reinforced plastic product gel coat for automobile parts and preparation method thereof |
CN111019494B (en) * | 2019-12-31 | 2021-10-01 | 南京德嘉玻璃钢材料有限公司 | High-weather-resistance gel coat and preparation method thereof |
CN113004600B (en) * | 2021-02-25 | 2022-11-15 | 浙江金菱制冷工程有限公司 | Cooling tower filler and preparation process thereof |
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