CN105036435A - Ammonia removal technique of aminoantipyrine ammonium sulfate mother solution - Google Patents
Ammonia removal technique of aminoantipyrine ammonium sulfate mother solution Download PDFInfo
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- CN105036435A CN105036435A CN201510313600.8A CN201510313600A CN105036435A CN 105036435 A CN105036435 A CN 105036435A CN 201510313600 A CN201510313600 A CN 201510313600A CN 105036435 A CN105036435 A CN 105036435A
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- 238000000034 method Methods 0.000 title claims abstract description 50
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 28
- RLFWWDJHLFCNIJ-UHFFFAOYSA-N 4-aminoantipyrine Chemical compound CN1C(C)=C(N)C(=O)N1C1=CC=CC=C1 RLFWWDJHLFCNIJ-UHFFFAOYSA-N 0.000 title claims abstract description 21
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052921 ammonium sulfate Inorganic materials 0.000 title claims abstract description 19
- 235000011130 ammonium sulphate Nutrition 0.000 title claims abstract description 19
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 15
- 239000010413 mother solution Substances 0.000 title abstract 4
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims abstract description 36
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000001105 regulatory effect Effects 0.000 claims abstract description 4
- 239000012452 mother liquor Substances 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- YZVWKHVRBDQPMQ-UHFFFAOYSA-N aminoantipyrene Natural products C1=C2C(N)=CC=C(C=C3)C2=C2C3=CC=CC2=C1 YZVWKHVRBDQPMQ-UHFFFAOYSA-N 0.000 claims description 17
- 238000009833 condensation Methods 0.000 claims description 13
- 230000005494 condensation Effects 0.000 claims description 12
- 238000012856 packing Methods 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- 230000009615 deamination Effects 0.000 claims description 8
- 238000006481 deamination reaction Methods 0.000 claims description 8
- 230000000694 effects Effects 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 230000010354 integration Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 10
- 229940120889 dipyrone Drugs 0.000 description 8
- DJGAAPFSPWAYTJ-UHFFFAOYSA-M metamizole sodium Chemical compound [Na+].O=C1C(N(CS([O-])(=O)=O)C)=C(C)N(C)N1C1=CC=CC=C1 DJGAAPFSPWAYTJ-UHFFFAOYSA-M 0.000 description 8
- 239000002351 wastewater Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 208000012639 Balance disease Diseases 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- -1 ammonium ions Chemical class 0.000 description 1
- 230000001754 anti-pyretic effect Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 231100000880 dysequilibrium Toxicity 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000000041 non-steroidal anti-inflammatory agent Substances 0.000 description 1
- 229940021182 non-steroidal anti-inflammatory drug Drugs 0.000 description 1
- 230000036284 oxygen consumption Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Physical Water Treatments (AREA)
Abstract
The invention relates to an ammonia removal technique of an aminoantipyrine ammonium sulfate mother solution, belonging to the technical field of effluent treatment in pharmacy industry. The technique comprises the following steps: the pH value of the mother solution is regulated, the mother solution is preheated and enters a high-pressure rectification tower to perform ammonia nitrogen removal, the feed material is preheated by a hot material stream on the tower bottom, 25% or so ammonia water is obtained from the tower top of the rectification tower, the tower top hot material stream can be completely condensed by circulating water, and the ammonia nitrogen content of the tower bottom effluent is less than 20 ppm. The whole process has the advantages of simple technique and small occupied area, is easy to implement, lowers the energy consumption by adopting the hot integration technique, and achieves the stable and efficient removal effect by using the lowest cost.
Description
[technical field]
The invention belongs to the drainage sunk well field of pharmaceutical industry, be specifically related to the technical process of aminoantipyrene ammonium sulfate liquor ammonia nitrogen removal.
[background technology]
Sulpyrine is a kind of antipyretic-antalgic and non_steroidal anti_inflammatory drug that grew up 20 beginnings of the century, and antipyretic effect is fast and strong.In the ammonium sulfate liquor of its production process intermediate aminoantipyrene, ammonia-nitrogen content exceeds standard, and is the waste water discharged after needing process.There is the outstanding problems such as quantity discharged is large, ammonia nitrogen concentration is high, and intractability is large in this waste water.
Directly entered in river, lake if nitrogenous effluent does not process, the eutrophication of water body can be caused, cause water ecology dysequilibrium.Ammonia nitrogen has very high oxygen-consumption, and cause water body to turn black smelly, deteriorating water quality, impacts the existence of aquatic animals and plants.The enterprises such as chemical industry, oil refining, chemical fertilizer, coking are the discharge rich anies influential family of high-concentration ammonia nitrogenous wastewater.National regulation, in waste discharge, ammonia-nitrogen content can not more than 25mg/L.
At present, the removal methods of ammonia nitrogen waste water has a variety of, as blow-off method, chemical precipitation method, break point chlorination method, film absorption technique etc.These methods all can reach certain removal effect, but there is a lot of problem.Blow-off method secondary pollution is serious, and stripping efficiency is low, has incrustation scale to generate in production process; Chemical precipitation method processing cost is high, and in waste water, ammonia nitrogen residual concentration is higher, and adding of medicament can pollute problem with sedimentary generation; In break point chlorination method to the use completely of liquid chlorine and shelf appeal high, processing cost is higher; In film absorption technique, the aqueous phase of film both sides is easy to seepage occurs under the effect of pressure reduction, and membrane separation process equipment cost is high, and occupied ground stock number is large, and equipment amortization is fast, and working cost is high.
Chinese patent 201110426110.0,201010123251.0 all mention vaporizing extract process ammonia nitrogen removal.Vaporizing extract process can reach good removal effect, but device is complicated, and floor space is large, and whole technical process needs multiple stage pump, if the pretreated waste water mordant solution that is high temperature, then require very high to device performance, cost is high.
What traditional ammonia nitrogen rectifying absorbed Ammonia Process processed employing is two towers operations, and floor space is large, and cost of investment is high.
Chinese patent 203602435U mentions atmospheric distillation ammonia nitrogen removal.Compared with the present invention, when identical feed conditions and rectifying tower basic parameter identical, high-pressure rectification removal effect is better, and energy consumption is low.
[summary of the invention]
Instant invention overcomes the deficiencies in the prior art, propose a kind of aminoantipyrene ammonium sulfate liquor deamination technique, efficient removal can be carried out to the high-concentration ammonia nitrogenous wastewater that concentration range is 3000-10000mg/L.
Technical scheme of the present invention is: a kind of aminoantipyrene ammonium sulfate liquor deamination technique, the steps include:
A. regulate mother liquor pH with NaOH, make pH>11, the mother liquor regulated directly enters preheater, through preheater preheats to 75-80 DEG C.
B. the mother liquor after preheating enters high-pressure rectification tower and carries out ammonia nitrogen removal in the middle part of tower.
C. high-pressure rectification tower tower reactor stream outlet is connected with preheater hot stream inlet, carries out preheating to charging, hot integrated saving energy consumption.
D. high-pressure rectification column overhead stream enters condenser system and carries out condensation, obtains high density ammoniacal liquor.
Owing to there is a large amount of ammonium ions in ammonia nitrogen mother liquor, regulate the mother liquor of pH value in the basic conditions after preheater preheats, ammonia is converted into molecularity by ionic condition, and reaches the requirement entering high-pressure rectification tower.After mother liquor enters high-pressure rectification tower, because the volatility of ammonia is greater than water, under the effect of steam, the ammonia in mother liquor proceeds to gas phase state.Through gas-liquid phase equilibrium repeatedly, amino molecule reaches the concentration requirement of design after separating with the state of ammonia steam, enter condenser system and liquefy, and obtains high density, high-quality ammoniacal liquor after entering multi-stage condensing.
Described condenser system comprises three grades of condensations, adopts circulating water, saves cost.
Described condenser, I and II is shell and tube cooler, easy to clean dirt; Three grades of condensers are plate-type condenser, and floor space is little, good effect of heat exchange.
Described high-pressure rectification tower packing layer height is less than 10m, and feed entrance point is in the middle part of high-pressure rectification tower, and working pressure is 2-10atm, and reflux ratio is 0.5-6.
The principle that the present invention realizes is:
As shown in Figure 1, the alkaline mother liquor regulating pH value, after preheater preheats is to 75-80 DEG C, enters high-pressure rectification tower by appropriate location in the middle part of tower, tower is divided into two sections, and epimere is rectifying section, and not containing charging, hypomere is stripping section containing feed plate.Utilize the difference of each component volatilization ability in mixture, by the backflow of liquid and gas, make gas, the reverse MULTI CONTACT of liquid two-phase, under the constraint of heat-driven and phase equilibrium relationship, volatile components (ammonia) is constantly shifted toward gas phase from liquid phase, and difficult volatiles is moved in liquid phase by gas phase, mixture is constantly separated.Finally, tower reactor logistics is discharged as the qualified mother liquor after process, and the hot logistics of tower top enters condenser system and carries out condensation.Regulate suitable reflux ratio and optimum working pressure, final rectifying tower tower top can obtain the high density ammoniacal liquor meeting industrial ammonia concentration requirement, and at the bottom of tower, draining ammonia-nitrogen content is far smaller than discharging standards.
The present invention has following beneficial effect:
(1) invention increases the removal effect of ammonia nitrogen in solution impurity.When adopting high-pressure rectification method removal of ammonia and nitrogen impurity, technique is simple, and energy consumption is low.Tower top can obtain the ammoniacal liquor that concentration is about 25%, meets industrial ammonia concentration requirement, and at the bottom of tower, draining ammonia-nitrogen content is less than 20ppm, and ammonia-nitrogen removal rate is close to 100%.Reach due technological effect well.
(2) what invention increases ammonia nitrogen in solution impurity removes stability, adopts continuous production technology, and avoid the fluctuation that in batch production process, between each batch, ammonia nitrogen impurity remains in the solution comparatively large, therefore treatment effect is stablized.
(3) the ammonia recycle that can reclaim of the present invention, improves economic benefit, different according to the annual treatment capacity of different factory, reclaims high density ammoniacal liquor hundreds of ton every year, by 400 yuan of calculating per ton, then obtains the extra returns of hundreds of thousands of every year.
(4) The present invention reduces the consumption of fresh water steam, reduce production cost.The present invention utilizes the hot logistics preheated feed of tower reactor.Be the technical process of 10t/h for treatment capacity, save steam about 4300 tons every year, amount to into expense about 950,000 yuan.
[accompanying drawing explanation]
Fig. 1 is the schema of aminoantipyrene ammonium sulfate liquor deamination technique of the present invention, wherein:
1-high-pressure rectification tower; 2-preheater; 3-condenser system; 4-mother liquor; Mother liquor after 5-preheating; The hot logistics of 6-tower reactor; 7-finally discharges mother liquor; The hot logistics of 8-tower top; Ammoniacal liquor after 9-condensation.
[embodiment]
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment is all carried out according to following steps: add alkali and be adjusted to pH>11, and by mother liquor preheating to be processed, enter high-pressure rectification tower and carry out ammonia nitrogen removal, high-pressure rectification tower packing layer height is less than 10m.
Embodiment 1: produce the aminoantipyrene ammonium sulfate liquor that 20t ammonia nitrogen concentration is 10000mg/L in Sulpyrine production process, add 2000 kilograms of NaOH adjust ph, inlet amount is 10t/h, completes process in 2 hours.In preheater, mother liquor is preheating to 80 DEG C by 35 DEG C, high-pressure rectification tower packing layer height is about 6m, from the charging of tower medium position, working pressure is the optimum pressure after within the scope of 2-10atm optimizes, and reflux ratio is the optimum value in 0.5-6, process rear tower top and obtain the ammoniacal liquor that concentration is 25%, tower top temperature is 58 DEG C, can by hot for tower top logistics total condensation with recirculated water, and in the mother liquor after the reason of tower bottom, ammonia-nitrogen content is detected as 19ppm.
Embodiment 2: produce the aminoantipyrene ammonium sulfate liquor that 10t ammonia nitrogen concentration is 10000mg/L in Sulpyrine production process, add 950 kilograms of NaOH adjust ph, inlet amount is 5t/h, completes process in 2 hours.In preheater, mother liquor is preheating to 78 DEG C by 33 DEG C, high-pressure rectification tower packing layer height is about 4m, from the charging of tower medium position, working pressure is the optimum pressure after within the scope of 2-10atm optimizes, and reflux ratio is the optimum value in 0.5-6, process rear tower top and obtain the ammoniacal liquor that concentration is 25.2%, tower top temperature is 60 DEG C, can by hot for tower top logistics total condensation with recirculated water, and in the mother liquor after the reason of tower bottom, ammonia-nitrogen content is detected as 17ppm.
Embodiment 3: produce the aminoantipyrene ammonium sulfate liquor that 20t ammonia nitrogen concentration is 6000mg/L in Sulpyrine production process, add 1900 kilograms of NaOH adjust ph, inlet amount is 10t/h, completes process in 2 hours.In preheater, mother liquor is preheating to 79 DEG C by 30 DEG C, high-pressure rectification tower packing layer height is about 6m, from the charging of tower medium position, working pressure is the optimum pressure after within the scope of 2-10atm optimizes, and reflux ratio is the optimum value in 0.5-6, process rear tower top and obtain the ammoniacal liquor that concentration is 24.9%, tower top temperature is 59.2 DEG C, can by hot for tower top logistics total condensation with recirculated water, and in the mother liquor after the reason of tower bottom, ammonia-nitrogen content is detected as 14ppm.
Embodiment 4: produce the aminoantipyrene ammonium sulfate liquor that 15t ammonia nitrogen concentration is 8000mg/L in Sulpyrine production process, add 1450 kilograms of NaOH adjust ph, inlet amount is 5t/h, completes process in 3 hours.In preheater, mother liquor is preheating to 80 DEG C by 35 DEG C, high-pressure rectification tower packing layer height is about 5m, from the charging of tower medium position, working pressure is the optimum pressure after within the scope of 2-10atm optimizes, and reflux ratio is the optimum value in 0.5-6, process rear tower top and obtain the ammoniacal liquor that concentration is 25.5%, tower top temperature is 61 DEG C, can by hot for tower top logistics total condensation with recirculated water, and in the mother liquor after the reason of tower bottom, ammonia-nitrogen content is detected as 15ppm.
Embodiment 5: produce the aminoantipyrene ammonium sulfate liquor that 18t ammonia nitrogen concentration is 5500mg/L in Sulpyrine production process, add 1800 kilograms of NaOH adjust ph, inlet amount is 6t/h, completes process in 3 hours.In preheater, mother liquor is preheating to 75 DEG C by 30 DEG C, high-pressure rectification tower packing layer height is about 5m, from the charging of tower medium position, working pressure is the optimum pressure after within the scope of 2-10atm optimizes, and reflux ratio is the optimum value in 0.5-6, process rear tower top and obtain the ammoniacal liquor that concentration is 25.2%, tower top temperature is 57.8 DEG C, can by hot for tower top logistics total condensation with recirculated water, and in the mother liquor after the reason of tower bottom, ammonia-nitrogen content is detected as 10ppm.
Embodiment 6: produce the aminoantipyrene ammonium sulfate liquor that 20t ammonia nitrogen concentration is 7500mg/L in Sulpyrine production process, add 2100 kilograms of NaOH adjust ph, inlet amount is 5t/h, completes process in 4 hours.In preheater, mother liquor is preheating to 80 DEG C by 35 DEG C, high-pressure rectification tower packing layer height is about 4m, from the charging of tower medium position, working pressure is the optimum pressure after within the scope of 2-10atm optimizes, and reflux ratio is the optimum value in 0.5-6, process rear tower top and obtain the ammoniacal liquor that concentration is 24.8%, tower top temperature is 58.9 DEG C, can by hot for tower top logistics total condensation with recirculated water, and in the mother liquor after the reason of tower bottom, ammonia-nitrogen content is detected as 12ppm.
Embodiment 7: produce the aminoantipyrene ammonium sulfate liquor that 10t ammonia nitrogen concentration is 3000mg/L in Sulpyrine production process, add 1000 kilograms of NaOH adjust ph, inlet amount is 5t/h, completes process in 2 hours.In preheater, mother liquor is preheating to 76 DEG C by 30 DEG C, high-pressure rectification tower packing layer height is about 4m, from the charging of tower medium position, working pressure is the optimum pressure after within the scope of 2-10atm optimizes, and reflux ratio is the optimum value in 0.5-6, process rear tower top and obtain the ammoniacal liquor that concentration is 25%, tower top temperature is 57.6 DEG C, can by hot for tower top logistics total condensation with recirculated water, and in the mother liquor after the reason of tower bottom, ammonia-nitrogen content is detected as 8ppm.
Claims (4)
1. an aminoantipyrene ammonium sulfate liquor deamination technique, is characterized in that: described processing step is as follows,
A. regulate mother liquor pH with NaOH, make pH>11, the mother liquor regulated directly enters preheater, through preheater preheats to 75-80 DEG C;
B. the mother liquor after preheating enters high-pressure rectification tower and carries out ammonia nitrogen removal in the middle part of tower;
C. high-pressure rectification tower tower reactor stream outlet is connected with preheater hot stream inlet, carries out preheating to charging;
D. high-pressure rectification column overhead stream enters condenser system and carries out condensation, obtains high density ammoniacal liquor.
2. aminoantipyrene ammonium sulfate liquor deamination technique according to claim 1, it is characterized in that: described high-pressure rectification tower packing layer height is less than 10m, feed entrance point is in the middle part of high-pressure rectification tower, and working pressure is 2-10atm, and reflux ratio is 0.5-6.
3. aminoantipyrene ammonium sulfate liquor deamination technique according to claim 1, it is characterized in that: condenser system comprises three grades of condensations, I and II condenser is shell and tube cooler, and three grades of condensers are plate-type condenser, adopts circulating water condensing.
4. aminoantipyrene ammonium sulfate liquor deamination technique according to claim 1, is characterized in that: high-pressure rectification column overhead ammonia concn about 25%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115849478A (en) * | 2022-10-28 | 2023-03-28 | 安徽华塑股份有限公司 | Ammonia nitrogen treatment process in water of acetylene purification system |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013165533A1 (en) * | 2012-05-04 | 2013-11-07 | Robert Hickey | Ammonium recovery methods |
| CN203602435U (en) * | 2013-12-05 | 2014-05-21 | 赖桂艳 | Resourceful treatment process system for extracting high-concentration ammonia water from ammonia-nitrogen wastewater |
| CN104355472A (en) * | 2014-10-28 | 2015-02-18 | 北京赛科康仑环保科技有限公司 | Inorganic ammonium salt-containing wastewater treatment system, treatment process and application of wastewater treatment system |
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2015
- 2015-06-10 CN CN201510313600.8A patent/CN105036435A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013165533A1 (en) * | 2012-05-04 | 2013-11-07 | Robert Hickey | Ammonium recovery methods |
| CN203602435U (en) * | 2013-12-05 | 2014-05-21 | 赖桂艳 | Resourceful treatment process system for extracting high-concentration ammonia water from ammonia-nitrogen wastewater |
| CN104355472A (en) * | 2014-10-28 | 2015-02-18 | 北京赛科康仑环保科技有限公司 | Inorganic ammonium salt-containing wastewater treatment system, treatment process and application of wastewater treatment system |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115849478A (en) * | 2022-10-28 | 2023-03-28 | 安徽华塑股份有限公司 | Ammonia nitrogen treatment process in water of acetylene purification system |
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Application publication date: 20151111 |