CN104130618A - Sustained-release treatment method of organic anti-mildew agent used on organic coating - Google Patents
Sustained-release treatment method of organic anti-mildew agent used on organic coating Download PDFInfo
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- CN104130618A CN104130618A CN201410323135.1A CN201410323135A CN104130618A CN 104130618 A CN104130618 A CN 104130618A CN 201410323135 A CN201410323135 A CN 201410323135A CN 104130618 A CN104130618 A CN 104130618A
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Abstract
The invention relates to the technical field of materials, and relates to a sustained-release treatment method of an organic anti-mildew agent used on an organic coating. The sustained-release treatment method comprises the following steps: (1) an organic anti-mildew agent and surfactant micelle solution is prepared; (2) an organic anti-mildew agent and layered double-metal hydroxides hybrid is prepared with a co-precipitation method; (3) an aging treatment is carried out; and (4) cleaning, drying and grinding are carried out, and obtained powder is added into a paint material. According to the invention, a existence form of a traditional organic anti-mildew agent in an organic coating is changed, such that anti-mildew agent release period can be effectively prolonged, organic coating high-efficiency anti-mildew period can be prolonged, and organic coating service life in environments with high temperature, high humidity and mildews can be prolonged. When the modified organic anti-mildew agent is used in a common organic coating which is prone to mildews, a high-efficiency anti-mildew period can be prolonged by more than 1 time. Also, with the method, reduced activity caused by a reaction between the anti-mildew agent and certain components of the coating can be inhibited. The anti-mildew agent has no adverse influences on organic coating protective performance, bonding performance, and the like.
Description
Technical field
The invention belongs to material technology field, relate to a kind of method of modifying of organic additive, further relate to a kind of organic mould inhibitor slowly-releasing treatment process for organic coating.
Background technology
Being coated with organic coating is the important measures of metallic corrosion protection.But the materials such as the oils that organic coating itself contains, ester class can directly be decomposed as source of nutrition by mould; and the oozy plurality of enzymes of mould-growth and organic acidity material can decompose some macromolecular compound and indirectly destroy organic coating, make its degraded or lose provide protection.In organic coating, adding organic mould inhibitor is the cost-effective mode that solves mould erosion problem.But often do not reach requirement in the stability of organic mould inhibitor and work-ing life, under severe rugged environment, easily occur decompose and separate out, cause the high-effect anti-mould phase of organic coating to shorten.Under the severe environment such as hot and humid, the high efficient protected phase of organic mould inhibitor is no more than 2 years conventionally.Therefore,, even added the organic coating of organic mould inhibitor, in its lifetime, still there is the hidden danger that corroded by mould.
Extend high-effect anti-mould phase of organic coating, on the one hand can be by the approach realization of organic synthesis novel substance, be fixed on and on polymer carrier, make polymkeric substance mould inhibitor by the polymerization of mould inhibitor monomeric compound or by mould inhibitor molecule.These class methods are studied often both at home and abroad at present, also prepared numerous novel mildew resistant products, but the molecular weight of this class material is generally larger, molecular chain length, adding proportion in organic coating is high, exists with organic coating and reacts and coating performance is affected to large problem.
The other approach of the high-effect anti-mould phase of prolongation organic coating is the good organic mould inhibitor of existing effect is carried out to slowly-releasing processing; by means such as physics are coated; when protection is provided; control its rate of release; both the impact of mould inhibitor on coating proper property can be reduced, and lasting anti-mold effect can be obtained again.These class methods also do not have bibliographical information in the research field of anti-mildew coating at present.
Layered double hydroxide is a kind of pharmaceutical carrier (nano container) with laminate structure, has important application in fields such as catalysis, ion-exchange/absorption, pharmacy, photochemistry.Slowly-releasing modification by layered double hydroxide to active substance, can suppress the migration of active substance, plays the effect of controlling active substance rate of release.But layered double hydroxide is in not yet application on organic mould inhibitor for organic coating at present.
" performance of organic coatings for corrosion resistance that contains tungsten salt inhibiter-layered double hydroxide " (LI Dan-Dan, WANG Fang-Yong, YU Xiang, et.al..Progress in Organic Coatings, 2011,71:302 – 309) literary composition introduced and utilized layered double hydroxide to be coated tungsten salt inhibiter, preparation WO
4 2-the method of/LDHs additive, this additive joins in epoxy coating, can improve the Corrosion Protection of coating.
" inserting antibiotic composite character and the controlled antibacterial behavior of Mg-Al layered double hydroxide " (WANG Yi, ZHANG Dun.Materials Research Bulletin, 2012,47 (11): 3185-3194) literary composition has been introduced the anion intercalated method in layered double hydroxide of 4 kinds of microbiotic such as benzoate, penicillin, has realized the slow release of microbiotic in NaCl solution.
Above-mentioned document has been applied to layered double hydroxide in the modification of the materials such as inorganic salt inhibiter, organic microbiotic, has realized their slow release in the media such as epoxy coating, NaCl solution.The treatment process that document relates to is not also suitable for 2,4,5,6-tetrachloro-1, non-ionic types such as 3-benzene dicarbonitrile, n-octyl group-isothiazolinone and be insoluble in the slowly-releasing processing of the organic mould inhibitor of organic coating of water.Only have after slowly-releasing is processed, the content of organic mould inhibitor in hybrid just has using value while being greater than 20%, and adopts aforesaid method processing, and in the hybrid obtaining, organic mould inhibitor content is less than 20%.
Summary of the invention
The object of the invention is to propose the organic mould inhibitor slowly-releasing treatment process for organic coating of a kind of not volatile, difficult migration and long service life.Technical solution of the present invention is, organic coating is 2,4,5,6-tetrachloro-1 with organic mould inhibitor, 3-benzene dicarbonitrile or n-octyl group-isothiazolinone, and its slowly-releasing treatment process is,
(1), the preparation of organic mould inhibitor and Free Energy of Surfactant Micelle Solution
First prepare organic mould inhibitor and organic solvent solution, organic mould inhibitor is dissolved in organic solvent completely, organic mould inhibitor concentration is 1～5mol/L, again anion surfactant is dispersed in deionized water, compound concentration is 20～100g/L surfactant-dispersed liquid, deionized water used in advance logical nitrogen is removed oxygen and carbonic acid gas, according to volume ratio 1:5～1:1, machine mould inhibitor and organic solvent solution and surfactant-dispersed liquid are being continued to mix and blend under logical nitrogen environment, temperature remains on 10～50 DEG C, until organic solvent volatilizees completely, obtain organic mould inhibitor/Free Energy of Surfactant Micelle Solution,
(2), coprecipitation method is prepared organic mould inhibitor and layered double hydroxide hybrid
Mg (the NO that preparation mol ratio is 2:1
3)
26H
2o and Al (NO
3)
39H
2o mixing solutions is added drop-wise in organic mould inhibitor and Free Energy of Surfactant Micelle Solution prepared by step 1 under mechanical stirring environment, and the amount of the mixing solutions of dropping, according to Al wherein
3+determine with the molar ratio of organic mould inhibitor in step 1, the two ratio is controlled at 0.5～1.5, in dropping process, utilizing the NaOH solution hierarchy of control pH of 2mol/L is 9～10, and pass into all the time nitrogen, and after dropwising, reaction 2～4h, temperature remains on 10～50 DEG C, finally obtains the suspension liquid that contains organic mould inhibitor and layered double hydroxide hybrid;
(3), burin-in process
Reacted suspension liquid is heated to 50～85 DEG C of burin-in process 20～50h;
(4), clean, be dried and grind
The suspension liquid obtaining with deionized water suction filtration, cleaning step 3, and at 50～85 DEG C vacuum-drying 10～30h, final grinding obtains organic mould inhibitor and layered double hydroxide hybrid powder, and in organic mould inhibitor and layered double hydroxide hybrid powder, organic mould inhibitor component content is 20～80%.
Described organic solvent refers to volatile and can effectively dissolve the organic solvent of organic mould inhibitor.
Described anion surfactant is Sodium dodecylbenzene sulfonate or sodium oleate.
Organic mould inhibitor of weight ratio 0.1～2% and layered double hydroxide hybrid powder are added in paint vehicle, stir, carry out application according to the related request of paint coating afterwards.
Described paint vehicle is alkyd varnish, amino paint or polyurethane paint.
The present invention has changed the existence form of traditional organic mould inhibitor in organic coating; do not affect that organic mould inhibitor adheres to mould and the restraining effect basis of growing on; effectively suppress migration and the volatilization of organic mould inhibitor molecule in coating; extend deenergized period; make mildew-resistant composition provide protection to organic coating more enduringly, thereby extended the high-effect anti-mould phase of coating and the work-ing life in high temperature, high humidity, mould environment.Test-results shows, through organic mould inhibitor of modification of the present invention, in the conventional organic coating of easy mildew, the high-effect anti-mould phase can be extended more than 1 times.In addition, the present invention can also reduce the possibility that organic mould inhibitor and organic coating composition react, suppress simultaneously mould inhibitor due to the coating ingredients activity decreased causing that reacts; The present invention not only has no adverse effect to barrier propterty, the bonding properties etc. of organic coating; and occur after local damage when organic coating; layered double hydroxide is inhibited to the acidifying of local corrosive environment, can slow down local corrosion germinating and the expansion of protected metal.
Embodiment
Below will be specifically described the present invention, but the present invention's scope required for protection is not limited to the described scope of embodiment.
Embodiment 1
Organic mould inhibitor adopts n-octyl group-isothiazolinone.Operate through slowly-releasing treatment process (1)～(4) respectively, preparation n-octyl group-isothiazolinone and layered double hydroxide hybrid powder, specific operation process is as follows:
The methanol solution 100ml of n-octyl group-isothiazolinone of preparation 3mol/L, and the sodium oleate dispersion liquid 200mL of 20g/L.The two is being continued to mix and blend under nitrogen environment, and temperature remains on 25 ± 2 DEG C, until methyl alcohol volatilizees completely, prepares n-octyl group-isothiazolinone and sodium oleate micellar solution.Mg (the NO that preparation contains 0.3mol
3)
26H
2al (the NO of O and 0.15mol
3)
39H
2o mixing solutions is added drop-wise in n-octyl group-isothiazolinone and sodium oleate micellar solution under mechanical stirring environment.In dropping process, utilizing the NaOH solution hierarchy of control pH of 2mol/L is 9～10, and passes into all the time nitrogen.After dropwising, reaction 2h, temperature remains on 25 ± 2 DEG C, obtains n-octyl group-isothiazolinone and layered double hydroxide hybrid suspension liquid.Reacted suspension liquid is heated to 85 DEG C of burin-in process 30h.With deionized water suction filtration, clean suspension liquid, and at 85 DEG C vacuum-drying 10h, in agate mortar, grind and obtain n-octyl group-isothiazolinone and layered double hydroxide hybrid powder.
The content that adopts UV-3600 type ultraviolet-visible spectrophotometer and calibration curve method to measure, calculate n-octyl group-isothiazolinone in n-octyl group-isothiazolinone and layered double hydroxide hybrid powder is 73.65%.
Embodiment 2
Organic mould inhibitor adopts n-octyl group-isothiazolinone.Operate through slowly-releasing treatment process (1)～(4) respectively, preparation n-octyl group-isothiazolinone and layered double hydroxide hybrid powder, and be applied in paint vehicle, specific operation process is as follows:
The acetone soln 100ml of n-octyl group-isothiazolinone of preparation 5mol/L, and the Sodium dodecylbenzene sulfonate dispersion liquid 500mL of 60g/L.The two is being continued to mix and blend under nitrogen environment, and temperature remains on 45 ± 2 DEG C, until acetone volatilizees completely, prepares n-octyl group-isothiazolinone and Micelles of Dodecyl Benzene Sodium Sulfonate solution.Mg (the NO that preparation contains 1mol
3)
26H
2al (the NO of O and 0.5mol
3)
39H
2o mixing solutions is added drop-wise in n-octyl group-isothiazolinone and Micelles of Dodecyl Benzene Sodium Sulfonate solution under mechanical stirring environment.In dropping process, utilizing the NaOH solution hierarchy of control pH of 2mol/L is 9～10, and passes into all the time nitrogen.After dropwising, reaction 4h, temperature remains on 25 ± 2 DEG C, obtains n-octyl group-isothiazolinone and layered double hydroxide hybrid suspension liquid.Reacted suspension liquid is heated to 70 DEG C of burin-in process 50h.With deionized water suction filtration, clean suspension liquid, and at 70 DEG C vacuum-drying 20h, in agate mortar, grind and obtain n-octyl group-isothiazolinone and layered double hydroxide hybrid powder.N-octyl group-the isothiazolinone of weight ratio 0.2% and layered double hydroxide hybrid powder are added in A04-60 amino baking enamel, stir, spray to afterwards LY12CZ aluminium alloy thick plate (100 × 50 × 15mm) surface of anodic oxidation treatment, film thickness approximately 20 μ m.
The content that adopts UV-3600 type ultraviolet-visible spectrophotometer and calibration curve method to measure, calculate n-octyl group-isothiazolinone in n-octyl group-isothiazolinone and layered double hydroxide hybrid powder is 58.3%.
Carry out laboratory mould test according to GJB150.10-1986 " military equipment envrionment test method mould test ", the fungus resistance energy of A04-60 amino baking enamel after inspection interpolation n-octyl group-isothiazolinone and layered double hydroxide hybrid powder.Test is penicillium funiculosum, aspergillus versicolor, aspergillus niger, flavus and Chaetomium globosum with bacterial classification.The single spore suspension concentration of each bacterial classification of preparation is every milliliter 10
6± 2 × 10
5individual spore.Each bacterial classification spore suspension equal-volume is mixed, be then inoculated into test sample and control sample surface in the mode of spraying.Mould test is carried out in mould test chamber (MJ-010 type), and test temperature is 25～30 DEG C, and test period is 84d (3 test period).
Mould test result is as follows: after adding n-octyl group-isothiazolinone and layered double hydroxide hybrid powder, A04-60 amino baking enamel is at the surperficial sign that does not all occur mould-growth of front 2 cycles (56d) of mould test, and mildew grade is 0 grade; When off-test (84d), there is micro-mould-growth in sample surfaces, and mildew grade is 1 grade.
Comparison example
Directly the n-octyl group-isothiazolinone of weight ratio 0.2% is added in A04-60 amino baking enamel, stir, spray to afterwards the LY12CZ aluminium alloy thick plate surface of anodic oxidation treatment, film thickness approximately 20 μ m.Carry out laboratory mould test according to GJB150.10-1986 " military equipment envrionment test method mould test ", test period is 84d (3 test period).Mould test result is as follows: the A04-60 amino baking enamel that adds n-octyl group-isothiazolinone occurs micro-mould-growth within the 1st cycle (28 days) of mould test, and mildew grade is 1 grade; After 2 test periods (56d), surperficial mildew grade is 2 grades; When off-test (84d), surperficial mildew is serious, and mildew grade is 4 grades.
Embodiment 3
Organic mould inhibitor adopts 2,4,5,6-tetrachloro-1,3-benzene dicarbonitrile.Operate through slowly-releasing treatment process (1)～(4) respectively, preparation 2,4,5,6-tetrachloro-1,3-benzene dicarbonitrile and layered double hydroxide hybrid powder, specific operation process is as follows:
2,4,5 of preparation 1mol/L, 6-tetrachloro-1, the methanol solution 100ml of 3-benzene dicarbonitrile, and the sodium oleate dispersion liquid 100mL of 100g/L.The two is being continued to mix and blend under nitrogen environment, and temperature remains on 15 ± 2 DEG C, until methyl alcohol volatilizees completely, prepares 2,4,5,6-tetrachloro-1,3-benzene dicarbonitrile and sodium oleate micellar solution.Mg (the NO that preparation contains 0.3mol
3)
26H
2al (the NO of O and 0.15mol
3)
39H
2o mixing solutions is added drop-wise to 2,4,5,6-tetrachloro-1 under mechanical stirring environment, in 3-benzene dicarbonitrile and sodium oleate micellar solution.In dropping process, utilizing the NaOH solution hierarchy of control pH of 2mol/L is 9～10, and passes into all the time nitrogen.After dropwising, reaction 3h, temperature remains on 15 ± 2 DEG C, obtains 2,4,5,6-tetrachloro-1,3-benzene dicarbonitrile and layered double hydroxide hybrid suspension liquid.Reacted suspension liquid is heated to 50 DEG C of burin-in process 40h.With deionized water suction filtration, clean suspension liquid, and at 50 DEG C vacuum-drying 30h, in agate mortar, grind and obtain 2,4,5,6-tetrachloro-1,3-benzene dicarbonitrile and layered double hydroxide hybrid powder.
Adopt UV-3600 type ultraviolet-visible spectrophotometer and calibration curve method to measure, calculate 2,4,5,6-tetrachloro-1, in 3-benzene dicarbonitrile and layered double hydroxide hybrid powder 2,4,5,6-tetrachloro-1, the content of 3-benzene dicarbonitrile is 27.43%.
Embodiment 4
Organic mould inhibitor adopts 2,4,5,6-tetrachloro-1,3-benzene dicarbonitrile.Operate through slowly-releasing treatment process (1)～(4) respectively, preparation 2,4,5,6-tetrachloro-1,3-benzene dicarbonitrile and layered double hydroxide hybrid powder, and be applied in paint vehicle, specific operation process is as follows:
2,4,5 of preparation 2mol/L, 6-tetrachloro-1, the acetone soln 100ml of 3-benzene dicarbonitrile, and the Sodium dodecylbenzene sulfonate dispersion liquid 200mL of 50g/L.The two is being continued to mix and blend under nitrogen environment, and temperature remains on 25 ± 2 DEG C, until acetone volatilizees completely, prepares 2,4,5,6-tetrachloro-1,3-benzene dicarbonitrile and Micelles of Dodecyl Benzene Sodium Sulfonate solution.Mg (the NO that preparation contains 0.4mol
3)
26H
2al (the NO of O and 0.2mol
3)
39H
2o mixing solutions is added drop-wise to 2,4,5,6-tetrachloro-1 under mechanical stirring environment, in 3-benzene dicarbonitrile and Micelles of Dodecyl Benzene Sodium Sulfonate solution.In dropping process, utilizing the NaOH solution hierarchy of control pH of 2mol/L is 9～10, and passes into all the time nitrogen.After dropwising, reaction 4h, temperature remains on 25 ± 2 DEG C, obtains 2,4,5,6-tetrachloro-1,3-benzene dicarbonitrile and layered double hydroxide hybrid suspension liquid.Reacted suspension liquid is heated to 80 DEG C of burin-in process 20h.With deionized water suction filtration, clean suspension liquid, and at 80 DEG C vacuum-drying 20h, in agate mortar, grind and obtain 2,4,5,6-tetrachloro-1,3-benzene dicarbonitrile and layered double hydroxide hybrid powder.By 2 of weight ratio 2%, 4,5,6-tetrachloro-1,3-benzene dicarbonitrile and layered double hydroxide hybrid powder add in black synthetic enamel (II type), stir, dip-coating afterwards, to LC4CS aluminium alloy test piece (50 × 50 × 2mm) surface of anodic oxidation treatment, is prevented dust and is solidified rear film thickness approximately 20 μ m.
Adopt UV-3600 type ultraviolet-visible spectrophotometer and calibration curve method to measure, calculate 2,4,5,6-tetrachloro-1, in 3-benzene dicarbonitrile and layered double hydroxide hybrid powder 2,4,5,6-tetrachloro-1, the content of 3-benzene dicarbonitrile is 34.49%.
Carry out laboratory mould test according to GJB150.10-1986 " military equipment envrionment test method mould test ", test period is 84d (3 test period).Mould test result is as follows: add 2,4,5,6-tetrachloro-1, after 3-benzene dicarbonitrile and layered double hydroxide hybrid powder, synthetic enamel is after the 1st cycle (28d) of mould test, and the sign of mould-growth does not appear in surface, and mildew grade is 0 grade; After the 2nd cycle (56d) of mould test, there is micro-mildew sign in surface, and mildew grade is 1 grade; After the 3rd cycle (84d) of mould test, there is obvious mildew sign in surface, and mildew grade is 2 grades.
Comparison example
Direct by 2,4,5 of weight ratio 2%, 6-tetrachloro-1,3-benzene dicarbonitrile adds in black synthetic enamel (II type), stirs, and dip-coating is afterwards to the LC4CS aluminium alloy print surface of anodic oxidation treatment, film thickness approximately 20 μ m.Carry out laboratory mould test according to GJB150.10-1986 " military equipment envrionment test method mould test ", test period is 84d (3 test period).Mould test result is as follows: after the 1st cycle (28d) of mould test, the sign of mould-growth does not appear in surface, and mildew grade is 0 grade; After the 2nd cycle (56d) of mould test, there is serious mildew phenomenon in surface, and mildew grade is 3 grades; After the 3rd cycle (84d) of mould test, surface is covered by mould substantially, and mildew grade is 4 grades.
Claims (5)
1. for an organic mould inhibitor slowly-releasing treatment process for organic coating, it is characterized in that, organic coating is 2,4,5,6-tetrachloro-1 with organic mould inhibitor, 3-benzene dicarbonitrile or n-octyl group-isothiazolinone, and its slowly-releasing treatment process is,
(1), the preparation of organic mould inhibitor and Free Energy of Surfactant Micelle Solution
First prepare organic mould inhibitor and organic solvent solution, organic mould inhibitor is dissolved in organic solvent completely, organic mould inhibitor concentration is 1～5mol/L, again anion surfactant is dispersed in deionized water, compound concentration is 20～100g/L surfactant-dispersed liquid, deionized water used in advance logical nitrogen is removed oxygen and carbonic acid gas, according to volume ratio 1:5～1:1, machine mould inhibitor and organic solvent solution and surfactant-dispersed liquid are being continued to mix and blend under logical nitrogen environment, temperature remains on 10～50 DEG C, until organic solvent volatilizees completely, obtain organic mould inhibitor/Free Energy of Surfactant Micelle Solution,
(2), coprecipitation method is prepared organic mould inhibitor and layered double hydroxide hybrid
Mg (the NO that preparation mol ratio is 2:1
3)
26H
2o and Al (NO
3)
39H
2o mixing solutions is added drop-wise in organic mould inhibitor and Free Energy of Surfactant Micelle Solution prepared by step 1 under mechanical stirring environment, and the amount of the mixing solutions of dropping, according to Al wherein
3+determine with the molar ratio of organic mould inhibitor in step 1, the two ratio is controlled at 0.5～1.5, in dropping process, utilizing the NaOH solution hierarchy of control pH of 2mol/L is 9～10, and pass into all the time nitrogen, and after dropwising, reaction 2～4h, temperature remains on 10～50 DEG C, finally obtains the suspension liquid that contains organic mould inhibitor and layered double hydroxide hybrid;
(3), burin-in process
Reacted suspension liquid is heated to 50～85 DEG C of burin-in process 20～50h;
(4), clean, be dried and grind
The suspension liquid obtaining with deionized water suction filtration, cleaning step (3), and at 50～85 DEG C vacuum-drying 10～30h, final grinding obtains organic mould inhibitor and layered double hydroxide hybrid powder, and in organic mould inhibitor and layered double hydroxide hybrid powder, organic mould inhibitor component content is 20～80%.
2. a kind of organic mould inhibitor slowly-releasing treatment process for organic coating according to claim 1, is characterized in that, described organic solvent refers to volatile and can effectively dissolve the organic solvent of organic mould inhibitor.
3. a kind of organic mould inhibitor slowly-releasing treatment process for organic coating according to claim 1, is characterized in that, described anion surfactant is Sodium dodecylbenzene sulfonate or sodium oleate.
Described in a claim 1 for the using method of organic mould inhibitor slowly-releasing treatment process of organic coating, it is characterized in that, organic mould inhibitor of weight ratio 0.1～2% and layered double hydroxide hybrid powder are added in paint vehicle, stir, carry out application according to the related request of paint coating afterwards.
5. the using method of the organic mould inhibitor slowly-releasing treatment process for organic coating according to claim 4, is characterized in that, described paint vehicle is alkyd varnish, amino paint or polyurethane paint.
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| CN109762445A (en) * | 2019-01-24 | 2019-05-17 | 江南大学 | Polyaniline/manganese sesquioxide managnic oxide/dual anticorrosive paint of epoxy resin tri compound and preparation method thereof |
| CN110607122A (en) * | 2019-09-23 | 2019-12-24 | 无锡新而奇化工科技有限公司 | Multifunctional self-repairing polyurethane mesh coating and preparation method thereof |
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| CN109762445A (en) * | 2019-01-24 | 2019-05-17 | 江南大学 | Polyaniline/manganese sesquioxide managnic oxide/dual anticorrosive paint of epoxy resin tri compound and preparation method thereof |
| CN110607122A (en) * | 2019-09-23 | 2019-12-24 | 无锡新而奇化工科技有限公司 | Multifunctional self-repairing polyurethane mesh coating and preparation method thereof |
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Application publication date: 20141105 |