CN104212396A - Photo-curable resin composition for repairing facing marble plank and preparation and using method of photo-curable resin composition - Google Patents
Photo-curable resin composition for repairing facing marble plank and preparation and using method of photo-curable resin composition Download PDFInfo
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Abstract
The invention relates to a photo-curable resin composition for repairing a facing marble plank. The photo-curable resin composition comprises the following components in percentage by total weight being 100%: 70-92% of epoxy acrylate or modified epoxy acrylate, 5-30% of reactive diluent, 0-10% of plasticizer, 0.1-3% of photoinitiator and 0-20% of filler The composition is used for spraying or scraping the surface of the plank, can be fast cured by being irradiated by an ultraviolet light source or sunlight to realize repair enhancement and has the characteristics of fast construction speed, energy conservation, good grinding and polishing effects and the like.
Description
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Technical field
The invention belongs to processing of stone light-cured epoxy CALCIUM ACRYLATE sizing agent, particularly facing marble slabs repairing light curing adhesive.
Background technology
Stone surface, through grinding and polishing process, reaches high glossiness, can be used for building facing.Stone of marble structure heterogeneity, many, the intensity difference of joint fissure and cavity, before grinding and polishing, normal employing resin surface coating curing, strengthens stone material top layer, fills surface, reduce the breakage in grinding and polishing, improve surface gloss.The resin used in prior art, a class is unsaturated polyester resin, this resin solidification speed, and intensity is higher, but color inhibition, loss of properties on aging, environmental pollution is heavier; One class is epoxy resin, this mechanical strength of resin is high, ageing-resistant performance good, but curing speed is slower, adopt hanger plate technique often to need 2-3 days just can enter grinding and polishing operation, affect production efficiency, when adopting production line balance, need heat and accelerate solidification, volatile matter effusion affects environment, too increases energy consumption, is necessary to improve.
Summary of the invention
Not enough for solving prior art, the present invention proposes following technical scheme:
Prepare a kind of light curing resin composition, two are contained to multiple unsaturated charcoal-charcoal double-strand in major ingredient molecule in described resin combination, cause through light trigger, there is Raolical polymerizable, form cross-linkable polymeric, in stone material joint fissure and hole, fill up cementing, realize stone material top layer and surperficial reinforcement.
Resin combination is for major ingredient with Epocryl or modified epoxy acrylic ester resin, it consists of Epocryl or modified epoxy acrylate resin 70 ~ 92%, reactive thinner 5-30%, softening agent 0-10%, light trigger 0.1 ~ 3%, filler 0 ~ 20%, is weight percentage, and each component sum is 100%.
The Epocryl used in the present invention by epoxy resin and acrylic or methacrylic acid when catalyzer and stopper exist, react at 80-130 DEG C and obtain for 3-8 hour, the mol ratio of epoxide group and acrylic or methacrylic acid is 1:0.8-1.2, catalyst levels is the 0.1-1% of reinforced gross weight, and stopper consumption is the 0.1-0.8% of reinforced gross weight.Acid number in product Epocryl≤10mg KOH/g, best≤5mg KOH/g.
The modified epoxy acrylic ester resin used in the present invention is mixed by the Epocryl obtained as stated above and urethane acrylate and/or polyester acrylic fat, wherein Epocryl consumption obtain after accounting for mixing more than 50% of modified epoxy acrylic ester weight resin.
Urethane acrylate requires functional group number >=2, acid number≤5mgKOH/ g, 25 DEG C of viscosity≤15000mpa.s, the UV8502 bis-functional polyurethane acrylate of the holy Chemical Co., Ltd. in Jinhua, preferred Shenzhen supply.
Polyester acrylate requires functional group number >=2, acid number≤5mgKOH/g, 25 DEG C of viscosity≤4000 mpa.s, the GF-3106 type color inhibition polyester acrylate of preferred Guangzhou Ming Yue trade Co., Ltd supply and GF-3110 type low-viscosity polyester CALCIUM ACRYLATE.
Preparing the raw materials used epoxy resin of Epocryl is bisphenol A-type Racemic glycidol ethers, bisphenol-f type glycidyl ether type epoxy resin, aliphatic epoxy resin cycloaliphatic epoxy resin or their mixture, require molecule epoxy group number >=2,25 DEG C of viscosity≤20000mpa.s, best≤10000mpa.s, preferentially select E-51, E-44 bisphenol A epoxide resin, GEFR170, YDF-161, YDF-165, YDF-170 bisphenol F epoxy resin, ERL-4205,4206 type cycloaliphatic epoxy resins, D.E.R.TM 732 series aliphatic epoxy resin.Catalyzer selects four butyl bromation amine, triphenylphosphine, diethylamine, triethylamine, triphenylphosphine; The stopper ST-1 of Resorcinol, 2,6 di t butyl phenol, p methoxy phenol, the supply of Jiashan Bel's optical material company limited selected by stopper, preferred ST-1, p methoxy phenol.
In light curing resin composition of the present invention, reactive thinner uses the esters of acrylic acid containing 1 ~ 4 acryloxy in molecule, as Viscoat 295,1,4-butylene glycol diacrylate, methacrylic acid ethylene glycol fat, tertiary amyl alcohol tetraacrylate, hexanediyl fat, Isodecyl fat, isobomyl acrylate fat, benzyl acrylate fat, also can use vinyl cyanide; Single acryloxy acrylate consumption in reactive thinner most preferably less than 40 % parts by weight.
In light curing resin composition of the present invention softening agent select dihydroxyphenyl propane, molecular weight lower than 600 polyethers, O-phthalic dibutyl ester.
In light curing resin composition of the present invention, light trigger selects that titanium is luxuriant, camphorquinone, hexa-aryl bi-imidazole, coumarone element, thioxanthone, benzil ketals class, consider that ornamental stone repairs the particular requirement sticking with glue agent color inhibition and deep layer photocuring, the preferred IRGACURE 184 of UV-light light curing agent, DAROCURE 1173, benzoin dimethylether/benzophenone combination; Visible ray light curing agent preferred two 2, the macromolecular photoinitiator KIP 150 that 6-difluoro-3-luxuriant titanium of pyrroles's phenyl two (GR-FMT, 784), isopropyl benzene luxuriant iron (II) six fluorine phosphorus acid Pu (IRGACURE 261), Ning Bodi company produce.
Filler in light curing resin composition of the present invention requires that granularity is little, and tackifying is little, can reduce the cure shrinkage of glued membrane, strengthens grindability, selects ultra-fine marble flour, silicon powder, Paris white, preferably select nanometer grade calcium carbonate powder, ultra-fine marble flour.
The preparation method of Photocurable resin composition of the present invention:
(1), the preparation of Epocryl
In the reactor of jacketed heating unit and opposing steam flow condenser, add epoxy resin, by catalyzer and
Stopper is dissolved in acrylic or methacrylic acid, and by its suction intake chute, start reactor agitator, chuck heat temperature raising, when being warming up to 80 ~ 120 DEG C, the acid of dropping acrylic or methacrylic, time for adding 0.5-2 hour, after dripping, regulate temperature in the kettle within the scope of 100-130 DEG C, continue reaction 2.5-6 hour, drip and terminate rear material sample of getting in still per hour and survey acid number, when acid number is less than 10mgKOH/g, when being preferably less than 5mgKOH/g, namely cool, temperature is down to 20-60 DEG C, enters lower operation.Play when reaction completes and is cooled to 20-60 only preferably fill nitrogen in a kettle. from starting agitator, keep nitrogen atmosphere, reduce the form and aspect of Epocryl.
(2), the preparation of light curing resin composition
At shielding visible ray and with in the workshop of red-light source illumination, the Epocryl prepared is dropped into reactor, open and stir, urethane acrylate is added by formula, polyester acrylate, be warming up to 50-100 DEG C, stir 0.5-2 hour, be cooled to 20-60 DEG C, add reactive thinner successively, softening agent, filler, light trigger, after adding raw material, regulate temperature of charge to 30 ~ 60 DEG C, continue stirring 1 ~ 3 hour, 0.5-1.5 hour is vacuumized under-0.080 ~-0.095MPa vacuum degree condition, stop stirring, eliminate vacuum, in still, material enters automatic packaging production line through 100 order filter-cloth filterings, use light tight packing material, obtain light curing resin composition of the present invention.
Light curing resin composition of the present invention uses in the following manner:
(1), in the mode of manual brushing, light curing resin composition is painted on marble slabs polished surface to be ground, brushing amount is within the scope of 100-1000g/ ㎡, thickness is even, wiping operation should be carried out in indoor red illumination region, after completing brushing, sheet material is pushed into outdoor reception visible-light curing, also can opens incandescent light or ultraviolet source photocuring on the spot.
(2), on automatic production line, design, install UV-light or incandescent light irradiated site, light curing resin composition is transferred to marble slabs machined surface with spraying or the pouring mode of scraping, and then enters irradiated site, sends automatic production line and enter lower operation after solidification.
Ultraviolet light polymerization time 5-60 second, incandescent light 6-30 minute set time, outdoor daylight 10-60 minute set time.
Light curing resin composition of the present invention is used for facing marble slabs repairing and reinforcing compared with the prior art, has the following advantages:
Curing speed is fast, increases substantially production efficiency;
Solidification process does not need heating, and curing reaction is mild, and volatile matter is few, realizes energy-saving and environmental protection;
In sheet material grinding and polishing process through repairing, breakage rate is little, and machined surface glossiness is high, color inhibition, freeze-thaw-, long service life.
Embodiment
Now citing further illustrates technical scheme of the present invention:
Embodiment 1
In the three neck glass flask that 500ml is with stirring and reflux exchanger, add epoxy resin E-54 188g, vinyl cyclohexene diepoxide ERL-4205 75g, drive agitator, fill nitrogen, be warming up to 90 DEG C, 0.5g triphenylphosphine will be dissolved with, the 129.6g vinylformic acid of 1.0g p methoxy phenol is loaded in reinforced bottle, even instillation flask, temperature controls within 1.5 hours, to drip off at 90-95 DEG C, is warming up to 115 DEG C, 115 DEG C of-118 DEG C of isothermal reactions 4 hours, in bottle, steam continued reaction through prolong backflow.From adding vinylformic acid, feeding per hour surveys acid number.Reaction terminates product in rear cooling bottle, and discharging when temperature is down to 40 DEG C also stops filling nitrogen, and obtain 392g product, viscosity, form and aspect, the acid number of sampling analysis product Epocryl, the results are shown in Table 1.
Light curing resin composition is prepared in the darkroom of red illumination.Take prepared Epocryl 140g and add 500ml three-necked flask, drive agitator, add urethane acrylate UV8205 25g, be warming up to 60 DEG C, stir after 40 minutes, add reactive thinner Viscoat 295 23g successively, isobornyl acrylate 7g, softening agent dihydroxyphenyl propane 10g, the ultra-fine marble flour 10g of light trigger DAROCURE 784 1.0g filler, stirring is continued 1.2 hours after adding raw material, then with 100 order filter-cloth filtering dischargings, use light tight container package, sampling simultaneously detects viscosity, thickness is 30 minutes sunshine of 4mm glue sample, the physical and mechanical properties of ultraviolet radiation sample after 45 seconds, repair the glossiness after facing marble slabs form grinding polishing.
The results are shown in Table 2
embodiment 2
When preparing Epocryl, the raw material used is bisphenol f type epoxy resin YDF-175, epoxy equivalent (weight) 170,25 DEG C of viscosity 2200mpa.s, 170g, vinyl cyclic ethylene diepoxide ERL-4205 75g, catalyst of triethylamine 1.0g, stopper ST-1 0.8g vinylformic acid 129.6g, operational condition is with embodiment 1, obtain Epocryl 372.5g, sampling analysis the results are shown in Table 1.
In the preparation of light curing resin composition, be raw materials usedly:
Prepared Epocryl 140g, polyester acrylate GF-3106 20g, reactive thinner tertiary amyl alcohol three CALCIUM ACRYLATE 24g, Isodecyl fat 11g, softening agent polyethers 10g, light trigger two 2,6-difluoro-3-luxuriant the titanium of pyrroles's phenyl two (GR-FMT, 784) 0.8g, not filled, all the other obtain light curing resin composition 204g with embodiment 2.
Said composition and through the sample of sun exposure after 20 minutes, detected result is in table 2.
embodiment 3
When preparing Epocryl, the raw material used is bisphenol A epoxide resin E-54 188 g, diisoamyl diene diepoxide (ERL-4269) 85g, catalyzer triphenylphosphine 0.8g, diethylamine 1.0g, methacrylic acid 153g, other conditions are with embodiment 1, obtain Epocryl 426g, sampling and testing, the results are shown in Table 1.
When preparing light curing resin composition of the present invention, Epocryl consumption is 172g, reactive thinner Isosorbide-5-Nitrae-butyleneglycol diacrylate fat 20g, benzyl acrylate 10g, plasticizer phthalic acid dioctyl ester 15g, light curing agent KIP 150 3g, not filled, other conditions, with embodiment 1, obtain light curing resin composition 204g, sampling detects resin combination and sample, the results are shown in Table 2.
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table 1 epoxy acrylate detected result
table 2 light curing resin composition and sample detected result
Claims (16)
1. one kind for facing marble slabs repair light curing resin composition and preparation, using method, it is characterized in that light curing resin composition is made up of the Epocryl of 70-92% or modified epoxy acrylic ester resin, the reactive thinner of 5-30%, 0-10% softening agent, the light trigger of 0.1-3%, the filler of 0-20%, be weight percentage, sum is 100%; After light trigger initiated polymerization, composition forms cross-linkable polymeric, fills up cementing, realize stone material top layer and surperficial reinforcement in the joint fissure and hole of facing marble slabs.
2. light curing resin composition according to claim 1 and preparation using method thereof, it is characterized in that described Epocryl is sour when catalyzer and stopper exist by epoxy resin, acrylic or methacrylic, react at 80-130 DEG C and obtain for 3-8 hour, the mol ratio of epoxide group and acrylic or methacrylic acid is 1:0.8-1.2, Epocryl acid number≤10mg KOH/g, is preferably less than 5mg KOH/g.
3. light curing resin composition according to claim 2 and preparation using method thereof, it is characterized in that epoxy resin selects dihydroxyphenyl propane, bisphenol-f type glycidyl ether type epoxy resin, aliphatic epoxy resin, cycloaliphatic epoxy resin or their mixture, molecule epoxy group number >=2,25 DEG C of viscosity≤20000mpa.s, best≤10000mpa.s.
4. light curing resin composition according to claim 2 and preparation using method thereof, is characterized in that catalyzer is Tetrabutyl amonium bromide, diethylamine, triethylamine, triphenylphosphine; Preferred triethylamine, triphenylphosphine.
5. light curing resin composition according to claim 2 and preparation using method thereof, is characterized in that stopper is Resorcinol, 2,6 one DI-tert-butylphenol compounds, p methoxy phenol, ST-1, preferred ST-1, p methoxy phenol.
6. light curing resin composition according to claim 1 and preparation using method thereof, it is characterized in that modified epoxy acrylic ester resin is mixed by described Epocryl and urethane acrylate and/or polyester acrylic fat, the weight that described Epocryl accounts for mixture is no less than 50%.
7. light curing resin composition according to claim 6 and preparation using method thereof, it is characterized in that urethane acrylate functional group number >=2, acid number≤5mgKOH/g, 25 DEG C of viscosity are less than 15000mpa.s.
8. light curing resin composition according to claim 6 and preparation using method thereof, it is characterized in that polyester acrylate functional group number >=2, acid number≤5mgKOH/g, 25 DEG C of viscosity are less than 2500mpa.s.
9. light curing resin composition according to claim 1 and preparation using method thereof, it is characterized in that reactive thinner uses the esters of acrylic acid containing 1-4 acryloxy in molecule, comprise tetramethylol methane tetraacrylate, pentaerythritol triacrylate, Viscoat 295,1,6 one hexanediyl esters, 1,4-butyleneglycol diacrylate acid esters, methacrylic acid glycol ester, hydroxyethyl methylacrylate, isodecyl acrylate, isobornyl acrylate, benzyl acrylate ester, also comprise vinyl cyanide; Single acryloxy acrylate consumption is most preferably less than 40% parts by weight.
10. light curing resin composition according to claim 1 and preparation using method, it is characterized in that softening agent select dihydroxyphenyl propane, dioctyl phthalate (DOP), molecular weight lower than 600 polyethers.
11. light curing resin compositions according to claim 1 and preparation using method thereof, it is characterized in that light trigger selects that titanium is luxuriant, camphorquinone, hexa-aryl bi-imidazole, coumarone element, thioxanthone, benzil ketals, the preferred IRGACURE 184 of ultraviolet light polymerization, DAROCURE 1173, benzoin dimethylether/benzophenone combination, visible-light curing selects two 2, the luxuriant titanium of 6-bis-fluoro-3-pyrroles phenyl two (GR-FMT, 784), isopropyl benzene luxuriant iron (II) six fluorine phosphorus acid Pu (IRGACURE 261), macromolecular photoinitiator KIP150.
12. light curing resin compositions according to claim 1 and preparation using method thereof, is characterized in that filler selects ultra-fine marble flour, silicon powder, Paris white, preferred ultra-fine marble flour, nano-calcium carbonate calcium powder.
13. light curing resin compositions according to claim 1 and preparation using method thereof, is characterized in that preparation method is:
(1) preparation of Epocryl
At jacketed heating unit, epoxy resin is added in the reactor of steam condensing reflux device, by catalyzer, stopper is dissolved in acrylic or methacrylic acid, chuck heat temperature raising, when in still, material rises to 80-120 DEG C, acrylic or methacrylic acid is dripped in still, time for adding 0.5-2 hour, drip rear adjustment temperature in the kettle within the scope of 100-130 DEG C, continue reaction 2.5-6 hour, dropping terminates to get for latter every 1 hour material in still and measures acid number, when acid number is less than 10mgKOH/g, cool when being preferably less than 5mgKOH/g to 30-60 DEG C, obtain described Epocryl, from start agitator play reaction complete be cooled to 30-60 DEG C time only, preferably fill nitrogen to reactor, keep nitrogen atmosphere, in order to reduce Epocryl form and aspect.
14.(2) the preparation of light curing resin composition
At shielding visible ray, use in the workshop of red-light source illumination and described Epocryl is dropped into reactor, open stirring, polyurethane acroleic acid fat is added by formula, polyester acrylic fat, be warming up to 50-100 DEG C, stir 0.5-2 hour, be cooled to 30-60 DEG C, add reactive thinner successively, softening agent, filler, light trigger, after adding, continue to stir 1-3 hour, 0.5-1.5 hour is vacuumized under-0.080 ~-0.095Mpa vacuum degree condition, stop stirring, eliminate vacuum, in still, material enters automatic packaging production line after 100 order filter-cloth filterings, light tight packaging vessel is used to pack, obtain light curing resin composition of the present invention.
15. light curing resin compositions according to claim 1 and preparation using method thereof, is characterized in that the using method of described light curing resin composition is:
(1), in the mode of manual brushing, light curing resin composition is painted on marble slabs polished surface to be ground, brushing amount is within the scope of 100-1000g/ ㎡, thickness is even, wiping operation should be carried out in indoor red illumination region, after completing brushing, sheet material is pushed into outdoor reception visible-light curing, also can opens incandescent light or ultraviolet source photocuring on the spot.
16.(2), on automatic production line, design, installation UV-light or incandescent light irradiated site, light curing resin composition is transferred to marble slabs machined surface with spraying or the pouring mode of scraping, and then enters irradiated site, sends automatic production line and enter lower grinding and polishing operation after solidification.
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| CN105315946A (en) * | 2015-11-23 | 2016-02-10 | 苏州盖德精细材料有限公司 | Epoxy acrylate UV adhesive and preparation method thereof |
| CN106085263A (en) * | 2016-07-21 | 2016-11-09 | 中国人民解放军陆军航空兵学院 | A kind of light curing resin composition quickly repaired for aircraft non-bearing eyelid covering |
| CN106187316A (en) * | 2016-06-30 | 2016-12-07 | 安徽智博新材料科技有限公司 | A kind of ceramic product photocuring healant |
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| WO2017008242A1 (en) * | 2015-07-14 | 2017-01-19 | Henkel IP & Holding GmbH | Monomeric and oligomeric resins for one drop fill sealant application |
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| CN106675484A (en) * | 2016-12-27 | 2017-05-17 | 上海普利特复合材料股份有限公司 | UV cured repairing material and preparation method thereof |
| CN106700891A (en) * | 2015-11-15 | 2017-05-24 | 惠州市长润发涂料有限公司 | LED curing repair undercoat paint |
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| CN110903769A (en) * | 2019-11-08 | 2020-03-24 | 华南农业大学 | Ultraviolet curing adhesive and preparation method and application thereof |
| CN110903799A (en) * | 2019-12-02 | 2020-03-24 | 武汉市科达云石护理材料有限公司 | Water-based light-cured stone decorative surface adhesive |
| CN111808567A (en) * | 2020-07-31 | 2020-10-23 | 肇庆福田化学工业有限公司 | Water-based light-curing adhesive for natural stone bottom mesh adhesive and preparation method thereof |
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| WO2022271585A1 (en) * | 2021-06-24 | 2022-12-29 | MORE Surface Care, LLC | Method and system for treating a calcium-based stone for corrosion and stain resistance |
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| WO2017008242A1 (en) * | 2015-07-14 | 2017-01-19 | Henkel IP & Holding GmbH | Monomeric and oligomeric resins for one drop fill sealant application |
| CN106700891A (en) * | 2015-11-15 | 2017-05-24 | 惠州市长润发涂料有限公司 | LED curing repair undercoat paint |
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| CN106187316A (en) * | 2016-06-30 | 2016-12-07 | 安徽智博新材料科技有限公司 | A kind of ceramic product photocuring healant |
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| CN106085263A (en) * | 2016-07-21 | 2016-11-09 | 中国人民解放军陆军航空兵学院 | A kind of light curing resin composition quickly repaired for aircraft non-bearing eyelid covering |
| CN106281176A (en) * | 2016-07-28 | 2017-01-04 | 孙涛 | A kind of windshield renovation agent and preparation method thereof |
| CN106281176B (en) * | 2016-07-28 | 2019-04-19 | 孙涛 | A kind of windshield renovation agent and preparation method thereof |
| CN106634789A (en) * | 2016-11-09 | 2017-05-10 | 东莞市贝特利新材料有限公司 | Ultraviolet light cured type adhesive and preparation method thereof |
| CN106675484A (en) * | 2016-12-27 | 2017-05-17 | 上海普利特复合材料股份有限公司 | UV cured repairing material and preparation method thereof |
| CN109609071A (en) * | 2018-12-07 | 2019-04-12 | 石狮华宝新材料工程有限公司 | A kind of light binding, preparation method and bolt anti-corrosion technique protected for the anti-corrosion leak-proof of bolt, enhancing |
| CN110668760A (en) * | 2019-11-05 | 2020-01-10 | 苏州金螳螂文化发展股份有限公司 | Stone for carving and preparation method thereof |
| CN110903769A (en) * | 2019-11-08 | 2020-03-24 | 华南农业大学 | Ultraviolet curing adhesive and preparation method and application thereof |
| CN110903799A (en) * | 2019-12-02 | 2020-03-24 | 武汉市科达云石护理材料有限公司 | Water-based light-cured stone decorative surface adhesive |
| CN111808567A (en) * | 2020-07-31 | 2020-10-23 | 肇庆福田化学工业有限公司 | Water-based light-curing adhesive for natural stone bottom mesh adhesive and preparation method thereof |
| CN112552854A (en) * | 2020-12-18 | 2021-03-26 | 山东万圣博化工有限公司 | Conductive adhesive and preparation method thereof |
| WO2022271585A1 (en) * | 2021-06-24 | 2022-12-29 | MORE Surface Care, LLC | Method and system for treating a calcium-based stone for corrosion and stain resistance |
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Application publication date: 20141217 |