CN105566105A - Production device and technology of 1,2-cyclohexanedicarboxylic acid diisobutyl ester - Google Patents
Production device and technology of 1,2-cyclohexanedicarboxylic acid diisobutyl ester Download PDFInfo
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Abstract
The invention relates to a production device and technology of 1,2-cyclohexanedicarboxylic acid diisobutyl ester. The device is provided with an esterification kettle, a neutralization kettle, a standing kettle, a washing pot, a dealcoholization kettle and a decoloring kettle which are connected through guiding pipes in sequence. An esterification tower is connected to the esterification kettle. The esterification tower, a condenser I and a water distributor are sequentially connected to form a closed loop. The water distributor, the standing kettle and the washing pot are each connected with a water collecting pot. The water collecting pots are connected with a distillation kettle. The distillation kettle is connected with an alcohol water collecting pot. The production technology comprises the steps of esterification, neutralization, washing, dealcoholization, decoloring and the like, a 100% monoester reaction and a 99.5% diester reaction are generated in a reaction kettle, the product yield is high, reaction conditions are mild, and no other impurities are generated; alcohol is recycled to be used as raw materials for secondary recycling, and the raw material utilization rate is high; alcohol-contained water generated by neutralization, washing and an oil-water separator is distilled through a distillation tower, a condensate is recycled, clean production is achieved, and a small amount of kettle residue liquid is collected for biochemical treatment and then drained when qualified.
Description
Technical field
The present invention relates to Organic Chemicals preparing technical field, specifically a kind of production equipment of 1,2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester and technique.
Background technology
Large-scale normal butane method maleic anhydride production many employings solvent absorption process.Relative to water absorption technique, solvent absorbing energy consumption is low, and yield is high, and quality is good, and equipment corrosion is little, and the cycle of operation is long.The solvent of China Maleic Anhydrite production and application has DIBE1,2-cyclohexane dioctyl phthalate diisobutyl ester and DBP dibutyl phthalate, and wherein DIBE is more satisfactory lyosorption.Be characterized in: boiling point is high, under service temperature, vapour pressure is less, and solvent loss is less, and chemical stability is good, viscosity small flow is good, extremely weak with the avidity of water, good with the affinity of cis-butenedioic anhydride, due to not minimum containing phenyl ring toxicity, shortcoming is that market value is high, needs from external import.DBP is also good cis-butenedioic anhydride lyosorption, but has phenyl ring, and containing toxicity, under service temperature, vapour pressure is slightly high, and solvent loss is greater than DIBE.Because DBP product volume is large, market value is low, the 0.3-0.4 only having DIBE price doubly, has price advantage in market competition.
Enterprise, in order to adapt to market competition, must reduce the procurement price of DIBE, does not have manufacturer because DIBE product is domestic, first needs domestic enterprise oneself can produce DIBE solvent.Through great efforts, domestic to have producer to develop with DIBP diisobutyl phthalate be raw material, produced the technique of DIBE, tentatively reduce DIBE cost by hydrogenation method.There are the following problems for DIBP hydrogenation technique:
1, the easy inactivation of hydrogenation catalyst, DBP raw material will carry out deep desulfuration process, and catalyzer, sweetening agent valency are expensive, and cost is high;
2, consume hydrogen, compressor power consumption, affect cost, remain high;
3, the product after hydrogenation, containing the trans DIBE isomer of 4-5%, affects quality;
4, the side reaction of DIBP hydrogenation is many, the magazins' layout difficulty that product contains;
5, mass difference is larger compared with imported product.
Design a better operational path and produce DIBE product, make energy consumption lower, yield is higher, better quality, to meet the needs of maleic anhydride production and market, becomes current problem demanding prompt solution.
Summary of the invention
The problems such as the cost existed for above-mentioned existing DIBE production technique is high, quality product difference compared with imported product is larger, the invention provides a kind of production equipment and technique of 1,2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of 1, the production equipment of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, this device be provided with connected in turn by conduit esterifying kettle, in and still, leave standstill still, water washing tank, dealcoholysis still and decolouring still, described esterifying kettle is also connected with esterification column, esterification column and condenser I and water trap are in turn connected to form loop line, described water trap, standing still and water washing tank are connected to water collecting tank, and described water collecting tank is all connected with still kettle, and still kettle is connected with alcohol water collecting tank.
Described dealcoholysis still is connected with condenser II through dealcoholize column, and condenser II is connected with recovery alcohol tank and solidifying water collecting tank respectively by Liang Ge branch.
Described decolouring still is connected with finished pot through activated charcoal filter.
Described esterifying kettle, in and still, leave standstill still, water washing tank, dealcoholysis still and decolouring still between connecting pipeline on be equipped with material pump.
One utilizes device as above to produce the method for 1,2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, comprises the following steps:
Step one: raw material HHPA and isopropylcarbinol are added esterifying kettle according to mol ratio 1:1-1:2, add catalyzer, be warming up to 60-150 DEG C of esterification 10-20h, the water vapor produced in reaction and isopropylcarbinol steam enter condenser I through esterification column, phlegma is isolated isopropylcarbinol and is returned esterifying kettle in water trap, and aqueous phase enters water collecting tank;
Step 2: during the esterifying liquid generated in esterifying kettle is sent into and in still, with alkali lye neutralization, then send into and leave standstill still stratification, water phase separated enters water collecting tank, and thick ester is sent in water washing tank and washed, and washing water are put in water collecting tank after being separated; Or in the esterifying liquid feeding generated in esterifying kettle and in still, with alkali lye neutralization, then send into and leave standstill still stratification, water phase separated enters water collecting tank, omission water-washing step; Or omission neutralization procedure, directly sent in water washing tank by the esterifying liquid generated in esterifying kettle and wash, washing water are put in water collecting tank after being separated;
Step 3: after washing, product is sent into dealcoholysis still and removed isopropylcarbinol, and after dealcoholysis, the product of gained is sent to decolouring still, through charcoal absorption decolouring, reaches the quality standard of finished product;
Step 4: by being sent to still kettle being heated to 90-120 DEG C containing alcohol water in water collecting tank in step one, step 2, alcohol-water azeotrope enters alcohol water collecting tank after condensation, then delivers to water washing tank recirculation and uses.
Deliver to activated charcoal filter removal activity carbon powder again through the finished product of charcoal absorption decolouring in described step 3, press filtration temperature of charge is 80-100 DEG C, and the finished product after decolouring sends into finished pot.
In described step one, catalyzer is methane cupric sulfophenate, tosic acid or 98%H
2sO
4, catalyst levels is: accounting for reaction raw materials molar percentage is 1%-2%.
Alkali lye in described step 2 is sodium hydroxide solution or Carbon Dioxide sodium solution, the consumption of alkali lye by the 20-30% of generation ester amount, the neutral temperature of alkali lye is 60 ~ 80 DEG C.
The temperature of washing in described step 2 is 60 ~ 80 DEG C, and water consumption is the 20-30% of ester amount.
In described step 3, material is heated to 60-80 DEG C in dealcoholysis still, dealcoholysis time 3 ~ 4h, through dealcoholize column, be no more than 145 DEG C in temperature ,-0.097 ~-0.0985MPa vacuum condition gasified, enters condenser II, phlegma is separated to enter and reclaims alcohol tank, non-condensable gas enters after vacuum buffer tank is separated lime set through refrigerated water interchanger and is extracted out by vacuum pump, and maintain system vacuum, lime set enters withdrawing can.
Beneficial effect of the present invention:
The production equipment of 1,2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester provided by the invention and technique, the monoesters reaction 100% that raw material produces in a kettle., dibasic acid esters reaction 99.5%, product yield is high; Raw material HHPA is called cis HHPA, product 100% cis after esterification, not containing trans-isomer(ide); Reaction conditions is mild, produces without other impurity; Reclaim alcohol as raw material secondary returning use, raw material availability is high; The alcohol water that contains of neutralization, washing, water-and-oil separator distills through distillation tower, lime set cyclically utilizing, cleaner production, and a small amount of still raffinate does the qualified discharge of biochemical treatment after collecting; Except raw material cost, processing charges is very low, and the total expenses of producing DIBE is only about the 0.3-0.4 of imported product, and can reach the same quality level of imported product.
Accompanying drawing explanation
Fig. 1 structural representation of the present invention;
Reference numeral: 1, esterifying kettle, 2, esterification column, 3, condenser I, 4, water trap, 5, solidifying water pot, 6, material pump I, 7, in and still, 8, material pump II, 9, leave standstill still, 10, water collecting tank I, 11, material pump III, 12, water washing tank, 13, water collecting tank II, 14, material pump IV, 15, alcohol Water Sproading pump, 16, dealcoholysis still, 17, dealcoholize column, 18, condenser II, 19, material pump V, 20, reclaim alcohol tank, 21, reclaim alcohol pump, 22, refrigerated water interchanger, 23, vacuum buffer tank, 24, solidifying water collecting tank, 25, vacuum pump, 26, decolouring still, 27, finished pot, 28, activated charcoal filter, 29, material pump VI, 30, still kettle, 31, distillation tower, 32, condenser III, 33, alcohol water collecting tank, 34, material pump VII, 35, raffinate holding tank.
Embodiment
Below in conjunction with embodiment, the present invention is further elaborated.
As shown in the figure: a kind of 1, the production equipment of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, this device is provided with the esterifying kettle 1 connected in turn by conduit, in and still 7, leave standstill still 9, water washing tank 12, dealcoholysis still 16 and decolouring still 26, described esterifying kettle 1 and in and connecting pipeline between still 7 be provided with material pump I 6, in and connecting pipeline between still 7 and standing still 9 be provided with material pump II 8, the connecting pipeline left standstill between still 9 and water washing tank 12 is provided with material pump III 11, connecting pipeline between water washing tank 12 and dealcoholysis still 16 is provided with material pump IV 14, connecting pipeline between dealcoholysis still 16 and decolouring still 26 is provided with material pump V 19, described esterifying kettle 1 is also connected with esterification column 2, esterification column 2 is in turn connected to form loop line with condenser I 3 and water trap 4, water trap 4 is also connected with solidifying water pot 5, leave standstill on still 9 and be connected with water collecting tank I 10, water washing tank 12 is connected with water collecting tank II 13, described solidifying water pot 5, water collecting tank I 10 and water collecting tank II 13 are all connected with still kettle 30, still kettle 30 is connected with condenser III 32 through distillation tower 31, condenser III 32 is connected with alcohol water collecting tank 33, alcohol water collecting tank 33 is connected with material pump VII 34, described dealcoholysis still 16 is connected with condenser II 18 through dealcoholize column 17, condenser II 18 is by Liang Ge branch, a branch is connected with recovery alcohol tank 20, reclaim on alcohol tank 20 and be connected with recovery alcohol pump 21, another branch is connected with vacuum buffer tank 23 by refrigerated water interchanger 22, and vacuum buffer tank 23 is connected with solidifying water collecting tank 24, vacuum buffer tank 23 is also connected with vacuum pump 25, and described decolouring still 26 is connected with finished pot 27 through activated charcoal filter 28, is provided with and expects pump VI 29 between decolouring still 26 and activated charcoal filter 28.
Embodiment 1
One utilizes device as above to produce the method for 1,2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, comprises the following steps:
Step one: raw material HHPA and isopropylcarbinol are added esterifying kettle 1 according to mol ratio 1:1, add catalyst methane cupric sulfophenate, its consumption is 1%% for accounting for reaction raw materials molar percentage, then 60 DEG C of esterification 10h are warming up to, the water vapor produced in reaction and isopropylcarbinol steam enter condenser I 3 through esterification column 2, phlegma is isolated isopropylcarbinol and is returned esterifying kettle 1 in water trap 4, and aqueous phase enters solidifying water pot 5;
Step 2: during the esterifying liquid generated in esterifying kettle 1 is sent into and in still 7, neutralize with alkali lye, described alkali lye is sodium hydroxide solution or Carbon Dioxide sodium solution, the consumption of alkali lye by generation ester amount 20%, the neutral temperature of alkali lye is 60 DEG C, then send into and leave standstill still 9 stratification, water phase separated enters water collecting tank I 10, and thick ester sends into washing in water washing tank 12, and the temperature of washing is 60 DEG C, water consumption is 20% of ester amount, and washing water are put in water collecting tank II 13 after being separated;
Step 3: after washing, product is sent into dealcoholysis still 16 and removed isopropylcarbinol, material is heated to 60 DEG C in dealcoholysis still 16, dealcoholysis time 3 ~ 4h, through dealcoholize column 17, is no more than 145 DEG C in temperature,-0.097MPa vacuum condition gasified, enter condenser II 18, phlegma is separated to enter and reclaims alcohol tank 20, and non-condensable gas enters after vacuum buffer tank 23 is separated lime set through refrigerated water interchanger 22 and extracted out by vacuum pump 25, maintain system vacuum, lime set enters withdrawing can 24; After dealcoholysis, the product of gained is sent to decolouring still 26, and through charcoal absorption decolouring, the finished product through charcoal absorption decolouring delivers to activated charcoal filter 28 removal activity carbon powder again, and press filtration temperature of charge is 80 DEG C, and the finished product after decolouring sends into finished pot 27;
Step 4: by being sent to still kettle 30 containing alcohol water and being heated to 90 DEG C in solidifying in step one, step 2 water pot 5, water collecting tank I 10 and water collecting tank II 13, alcohol-water azeotrope enters alcohol water collecting tank 33 after condensation, then delivers to water washing tank 12 recirculation and uses.
Embodiment 2
One utilizes device as above to produce the method for 1,2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, comprises the following steps:
Step one: raw material HHPA and isopropylcarbinol are added esterifying kettle 1 according to mol ratio 1:1.5, add catalyzer toluenesulphonic acids, its consumption is 1.5% for accounting for reaction raw materials molar percentage, then 100 DEG C of esterification 15h are warming up to, the water vapor produced in reaction and isopropylcarbinol steam enter condenser I 3 through esterification column 2, phlegma is isolated isopropylcarbinol and is returned esterifying kettle 1 in water trap 4, and aqueous phase enters solidifying water pot 5;
Step 2: during the esterifying liquid generated in esterifying kettle 1 is sent into and in still 7, neutralize with alkali lye, described alkali lye is sodium hydroxide solution or Carbon Dioxide sodium solution, the consumption of alkali lye by generation ester amount 25%, the neutral temperature of alkali lye is 70 DEG C, then send into and leave standstill still 9 stratification, water phase separated enters water collecting tank I 10, and thick ester sends into washing in water washing tank 12, and the temperature of washing is 70 DEG C, water consumption is 25% of ester amount, and washing water are put in water collecting tank II 13 after being separated;
Step 3: after washing, product is sent into dealcoholysis still 16 and removed isopropylcarbinol, material is heated to 70 DEG C in dealcoholysis still 16, dealcoholysis time 3 ~ 4h, through dealcoholize column 17, is no more than 145 DEG C in temperature,-0.098MPa vacuum condition gasified, enter condenser II 18, phlegma is separated to enter and reclaims alcohol tank 20, and non-condensable gas enters after vacuum buffer tank 23 is separated lime set through refrigerated water interchanger 22 and extracted out by vacuum pump 25, maintain system vacuum, lime set enters withdrawing can 24; After dealcoholysis, the product of gained is sent to decolouring still 26, and through charcoal absorption decolouring, the finished product through charcoal absorption decolouring delivers to activated charcoal filter 28 removal activity carbon powder again, and press filtration temperature of charge is 90 DEG C, and the finished product after decolouring sends into finished pot 27;
Step 4: by being sent to still kettle 30 containing alcohol water and being heated to 100 DEG C in solidifying in step one, step 2 water pot 5, water collecting tank I 10 and water collecting tank II 13, alcohol-water azeotrope enters alcohol water collecting tank 33 after condensation, then delivers to water washing tank 12 recirculation and uses.
Embodiment 3
One utilizes device as above to produce the method for 1,2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, comprises the following steps:
Step one: raw material HHPA and isopropylcarbinol are added esterifying kettle 1 according to mol ratio 1:2, adds catalyzer 98%H
2sO
4its consumption is 2% for accounting for reaction raw materials molar percentage, is then warming up to 150 DEG C of esterification 20h, and the water vapor produced in reaction and isopropylcarbinol steam enter condenser I 3 through esterification column 2, phlegma is isolated isopropylcarbinol and is returned esterifying kettle 1 in water trap 4, and aqueous phase enters solidifying water pot 5;
Step 2: during the esterifying liquid generated in esterifying kettle 1 is sent into and in still 7, neutralize with alkali lye, described alkali lye is sodium hydroxide solution or Carbon Dioxide sodium solution, the consumption of alkali lye by generation ester amount 30%, the neutral temperature of alkali lye is 80 DEG C, then send into and leave standstill still 9 stratification, water phase separated enters water collecting tank I 10, and thick ester sends into washing in water washing tank 12, and the temperature of washing is 80 DEG C, water consumption is 30% of ester amount, and washing water are put in water collecting tank II 13 after being separated;
Step 3: after washing, product is sent into dealcoholysis still 16 and removed isopropylcarbinol, material is heated to 80 DEG C in dealcoholysis still 16, dealcoholysis time 3 ~ 4h, through dealcoholize column 17, is no more than 145 DEG C in temperature,-0.0985MPa vacuum condition gasified, enter condenser II 18, phlegma is separated to enter and reclaims alcohol tank 20, and non-condensable gas enters after vacuum buffer tank 23 is separated lime set through refrigerated water interchanger 22 and extracted out by vacuum pump 25, maintain system vacuum, lime set enters withdrawing can 24; After dealcoholysis, the product of gained is sent to decolouring still 26, and through charcoal absorption decolouring, the finished product through charcoal absorption decolouring delivers to activated charcoal filter 28 removal activity carbon powder again, and press filtration temperature of charge is 100 DEG C, and the finished product after decolouring sends into finished pot 27;
Step 4: by being sent to still kettle 30 containing alcohol water and being heated to 120 DEG C in solidifying in step one, step 2 water pot 5, water collecting tank I 10 and water collecting tank II 13, alcohol-water azeotrope enters alcohol water collecting tank 33 after condensation, then delivers to water washing tank 12 recirculation and uses.
The object of washing removes alkali residual in oil phase, prevents product saponification value from exceeding standard, if acid number returns liter after washing, need mend alkali, to meet the Con trolling index of acid number.If it is enough good to obtain with process relativity in alkali lye, can skip washing step, directly enter dealcoholysis operation; Or the finished product skipping washing step still can meet quality index, then can directly enter dealcoholysis operation; When caustic wash process concentration of lye is higher or acid number is higher, washing often can not be omitted.
The monoesters reaction 100% that raw material of the present invention produces in a kettle., dibasic acid esters reaction 99.5%, product yield is high; Raw material HHPA is called cis HHPA, product 100% cis after esterification, not containing trans-isomer(ide); Reaction conditions is mild, produces without other impurity; Reclaim alcohol as raw material secondary returning use, raw material availability is high; The alcohol water that contains of neutralization, washing, water-and-oil separator distills through distillation tower, lime set cyclically utilizing, cleaner production, and a small amount of still raffinate does the qualified discharge of biochemical treatment after collecting; Except raw material cost, processing charges is very low, and the total expenses of producing DIBE is only about the 0.3-0.4 of imported product, and can reach the same quality level of imported product.
Claims (10)
1. the production equipment of a 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, it is characterized in that: this device is provided with the esterifying kettle (1) connected in turn by conduit, in and still (7), leave standstill still (9), water washing tank (12), dealcoholysis still (16) and decolouring still (26), described esterifying kettle (1) is also connected with esterification column (2), esterification column (2) is in turn connected to form loop line with condenser I (3) and water trap (4), described water trap (4), standing still (9) and water washing tank (12) are connected to water collecting tank, described water collecting tank is all connected with still kettle (30), still kettle (30) is connected with alcohol water collecting tank (33).
2. as claimed in claim 11, the production equipment of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, it is characterized in that: described dealcoholysis still (16) is connected with condenser II (18) through dealcoholize column (17), condenser II (18) is connected with recovery alcohol tank (20) and solidifying water collecting tank (24) respectively by Liang Ge branch.
3. the production equipment of 1,2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester as claimed in claim 1, is characterized in that: described decolouring still (26) is connected with finished pot (27) through activated charcoal filter (28).
4. as claimed in claim 11, the production equipment of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, is characterized in that: described esterifying kettle (1), in and still (7), leave standstill between still (9), water washing tank (12), dealcoholysis still (16) and decolouring still (26) connecting pipeline on be equipped with material pump.
5. the method utilizing device as claimed in claim 1 to produce 1,2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, is characterized in that, comprise the following steps:
Step one: raw material HHPA and isopropylcarbinol are added esterifying kettle (1) according to mol ratio 1:1-1:2, add catalyzer, be warming up to 60-150 DEG C of esterification 10-20h, the water vapor produced in reaction and isopropylcarbinol steam enter condenser I (3) through esterification column (2), phlegma is isolated isopropylcarbinol and is returned esterifying kettle (1) in water trap (4), and aqueous phase enters water collecting tank;
Step 2: during the esterifying liquid generated in esterifying kettle (1) is sent into and in still (7), with alkali lye neutralization, then send into and leave standstill still (9) stratification, water phase separated enters water collecting tank, thick ester sends into washing in water washing tank (12), and washing water are put in water collecting tank after being separated;
Step 3: after washing, product is sent into dealcoholysis still (16) and removed isopropylcarbinol, and after dealcoholysis, the product of gained is sent to decolouring still (26), through charcoal absorption decolouring, reaches the quality standard of finished product;
Step 4: by being sent to still kettle (30) being heated to 90-120 DEG C containing alcohol water in water collecting tank in step one, step 2, alcohol-water azeotrope enters alcohol water collecting tank (33) after condensation, then delivers to water washing tank (12) recirculation and uses.
6. production 1 as claimed in claim 5, the method of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, it is characterized in that: in described step 3, deliver to activated charcoal filter (28) removal activity carbon powder again through the finished product of charcoal absorption decolouring, press filtration temperature of charge is 80-100 DEG C, and the finished product after decolouring sends into finished pot (27).
7. method of producing 1,2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester as claimed in claim 5, is characterized in that: in described step one, catalyzer is methane cupric sulfophenate, tosic acid or 98%H
2sO
4, catalyst levels is: accounting for reaction raw materials molar percentage is 0.2%-2%.
8. production 1 as claimed in claim 5, the method of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, it is characterized in that: the alkali lye in described step 2 is sodium hydroxide solution or Carbon Dioxide sodium solution, the consumption of alkali lye by the 20-30% of generation ester amount, the neutral temperature of alkali lye is 60 ~ 80 DEG C.
9. method of producing 1,2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester as claimed in claim 5, it is characterized in that: the temperature of washing in described step 2 is 60 ~ 80 DEG C, water consumption is the 20-30% of ester amount.
10. production 1 as claimed in claim 5, the method of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, it is characterized in that: in described step 3, material is heated to 60-80 DEG C in dealcoholysis still (16), dealcoholysis time 3 ~ 4h, through dealcoholize column (17), 145 DEG C are no more than in temperature,-0.097 ~-0.0985MPa vacuum condition gasified, enter condenser II (18), phlegma is separated to enter and reclaims alcohol tank (20), non-condensable gas enters after vacuum buffer tank (23) is separated lime set through refrigerated water interchanger (22) and is extracted out by vacuum pump (25), maintain system vacuum, lime set enters withdrawing can (24).
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| CN115724879A (en) * | 2022-11-29 | 2023-03-03 | 泰安亚荣生物科技有限公司 | Production method and production equipment of flame retardant TCEP |
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Application publication date: 20160511 |