CN103752285B - Absorbent material for water body purification and biological carbon brick - Google Patents
Absorbent material for water body purification and biological carbon brick Download PDFInfo
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- CN103752285B CN103752285B CN201410008599.3A CN201410008599A CN103752285B CN 103752285 B CN103752285 B CN 103752285B CN 201410008599 A CN201410008599 A CN 201410008599A CN 103752285 B CN103752285 B CN 103752285B
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- 239000000463 material Substances 0.000 title claims abstract description 50
- 239000011449 brick Substances 0.000 title claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 14
- 229910052799 carbon Inorganic materials 0.000 title abstract description 14
- 238000000746 purification Methods 0.000 title abstract description 9
- 239000002250 absorbent Substances 0.000 title abstract description 7
- 230000002745 absorbent Effects 0.000 title abstract description 7
- 238000009792 diffusion process Methods 0.000 claims abstract description 29
- 239000010410 layer Substances 0.000 claims abstract description 24
- 101150096185 PAAS gene Proteins 0.000 claims abstract description 20
- 239000003344 environmental pollutant Substances 0.000 claims abstract description 15
- 231100000719 pollutant Toxicity 0.000 claims abstract description 15
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims abstract description 8
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000011229 interlayer Substances 0.000 claims abstract description 7
- 239000003610 charcoal Substances 0.000 claims description 29
- 239000000446 fuel Substances 0.000 claims description 28
- 239000012528 membrane Substances 0.000 claims description 27
- 230000004888 barrier function Effects 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 15
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000003431 cross linking reagent Substances 0.000 claims description 14
- 238000001179 sorption measurement Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 229920000936 Agarose Polymers 0.000 claims description 9
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 4
- 239000000017 hydrogel Substances 0.000 claims description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 7
- 230000001681 protective effect Effects 0.000 abstract 1
- 229910001385 heavy metal Inorganic materials 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000010815 organic waste Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000010828 animal waste Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 238000005899 aromatization reaction Methods 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- -1 stalk Substances 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Solid Fuels And Fuel-Associated Substances (AREA)
Abstract
The invention relates to an absorbent material for water body purification and a biological carbon brick; the absorbent material disclosed by the invention is composed of biological carbon and sodium polyacrylate (PAAS); the concentration of the PAAS solution is 0.1-50g/L; 10-200 g of biological carbon is added into 500-1000 mL of PAAS solution; the biological carbon brick comprises a hollow base; an annular top cover is installed on the top end of the base; the absorbent material is filled in the base; two layers of protective filter films cover the upper surface of the absorbent material; and a diffusion film interlayer is arranged between the two layers of filter films. According to the invention, due to the added diffusion film, PAAS and biological carbon can be effectively prevented from being dissolved; pollutants having high activity and low molecular weight are allowed to freely diffuse to enter the biological carbon brick, and therefore, the absorbent material for water body purification and the biological carbon brick disclosed by the invention have the capability of selectively eliminating hazard pollutants in a water body.
Description
Technical field
The invention belongs to environmental science, relate to the sorbing material for water body purification, especially a kind of for water body purification sorbing material and biological brick fuel.
Background technology
Charcoal typically refers to based on the biomass resource that extensively exists by nature, utilizes specific charring process, by the living beings carbonaceous that produces of imperfect combustion under anoxic conditions.Common charcoal comprises charcoal, bamboo charcoal, stalk, charcoal rice, shell charcoal etc.They, primarily of aromatic hydrocarbon and simple substance carbon or the carbon composition with graphite-structure, containing the carbon of more than 60%, also comprise H, O, N, S and a small amount of trace element.Charcoal has that raw material sources is extensive, production cost is low, ecological safety is pollution-free, can the distinguishing feature such as spread.
Charcoal solubility is extremely low, there is height carboxylic esterification and aromatization structure, have larger porosity and specific area, these fundamental propertys absorption affinity resistance to oxidation that made it possess and the strong characteristic of antibiont capacity of decomposition, can be widely used in removing the organic and inorganic pollution in water.
Charcoal is owing to having larger porosity, specific area, it is made to have great advantage on Adsorption of Heavy Metals and organic pollution, but because biological carbon is the black puffy solid matter that particle is careful, quality is lighter, charcoal after process is not easily separated from water body, and this shortcoming limits the application of charcoal.
Sodium Polyacrylate is-kind of water-soluble high-molecular compound, water soluble forms thick liquid, to the heavy metal in water body particularly bivalent metal ion have superpower sequestering power, but because Sodium Polyacrylate after the restriction chelating of content of beary metal is still water miscible, cannot be removed, be limited the application of Sodium Polyacrylate as water treatment agent.
Endangering larger in water body is active pollutant, active pollutant is as ionic state heavy metal, agricultural chemicals, low molecule POPs etc. can produce direct harm to biological and ecological environment, eliminating and processing active pollutant in water body is problem in urgent need to solve, and at present can the material of Adsorption water body high activity pollutant to there is adsorption capacity low, preparation cost compared with high, preparation difficulty is large, the follow-up shortcoming such as difficult, use is restricted.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, provide that a kind of material is novel, cost is low, advantages of good adsorption effect for water body purification sorbing material and biological brick fuel.
The technical scheme that the present invention realizes object is as follows:
A kind of for water body purification sorbing material, the solution that described material is formed by charcoal and Sodium Polyacrylate, the concentration of described PAAS is at 0.1-50g/L, and the content of described charcoal is 20-400g/L.
And described polyacrylic molecular weight is 3,000 ten thousand.
And the preparation method of described sorbing material is: first prepare PAAS solution, PAAS solution is joined in charcoal, mixes pressing and get final product.
A kind of biological brick fuel of sorbing material; comprise sorbing material and shell; sorbing material is filled in shell; sorbing material has exposed surface relative to shell; three metafiltration films are sealed at the exposed surface of sorbing material; described three metafiltration films are inside and outside two-layer protection filter membrane, between inside and outside two-layer protection filter membrane, arrange Pollutants Diffusion film interlayer.
And; the concrete structure of described biological brick fuel is: comprise a hollow base, installs ring-type top cover, filling adsorption material in base on base top; the upper surface of sorbing material covers inside and outside two-layer protection filter membrane, arranges Pollutants Diffusion film interlayer between two-layer filter membrane.
And it is 0.15-0.22 μm through the molecular weight 50-1000000 of material, the aperture of outer layer protection filter membrane that described diffusion barrier allows free, internal layer protection filter sizes 0.3-0.45 μm.
And the thickness of described diffusion barrier is 0.8mm, the thickness of inside and outside layer protection filter membrane is 0.1mm.
And, the preparation method of described diffusion barrier is: by acrylamide, crosslinking agent, ammonium persulfate, N, N, the hydrogel that-methylene-bisacrylamide is made, its preparation method is: acrylamide solution, crosslinking agent, high purity water are mixed, and adds ammonium persulfate, N successively, N,-methylene-bisacrylamide, pours into after mixing in mould, and acquisition aquagel membrane is diffusion barrier.
And the preparation method of described crosslinking agent is: in the allyl glycidyl ether added by sodium borohydride, obtain solution A; Agarose is added in NaOH solution, constantly stir and form agarose suspension B; Solution A is added in suspension B and form solution C, solution C is stirred 12h continuously; Mixed liquor is filtered, is washed till neutrality with distilled water; Dehydration, vacuum drying, obtains required crosslinking agent, described sodium borohydride: allyl glycidyl ether: agarose: NaOH weight ratio=0.2-0.4:9-20:5-15:3.6-6.
And described diffusion barrier is by acrylamide, crosslinking agent, ammonium persulfate, N, N, the hydrogel that-methylene-bisacrylamide is made.
Beneficial effect of the present invention and good effect as follows:
1, selected in the present invention Sodium Polyacrylate (PAAS) is the macromolecular compound of a kind of wire, solubility, carboxyl on its strand is due to electrostatic repulsion effect, the polymer chain circumnutated is stretched, facilitates the functional group with adsorptivity to be exposed to surface.Its structural formula is-[-CH2CHCOONa-]-, its functional group is that carboxyl preferably complex reaction can occur with metal ion.Because PAAS belongs to water-soluble organic high molecular compound, and wrapped up with diffusion barrier, it can be avoided from biological brick fuel stripping, solve the problem that PAAS is not suitable for being directly used in wastewater treatment.
2, the present invention is directed to charcoal and remove not segregative shortcoming after pollutant, prepare a kind solid biologic brick fuel, for the problem that the adsorption capacity of charcoal heavy metal is lower, add the heavy metal absorbents such as PAAS, add the adsorption capacity of charcoal heavy metal.
3, after the inner filling adsorption material of biological brick fuel provided by the invention, water body high activity pollutant can be removed, also have adsorption capacity high, applied widely, without unwanted particles stripping, adsorption efficiency advantages of higher.
4, the diffusion barrier added in the present invention effectively can prevent PAAS or other materials stripping, and optionally separating active substances, make this invention have the ability endangering large pollutant in selective removal water body.
5, biological brick fuel provided by the invention has the ability efficiently removing activity, low molecule organic matter, inorganic pollution, solves the dispersiveness of charcoal to such an extent as to irretrievable shortcoming, and sorbing material can be directly used in landfill or burning disposal after using.
Accompanying drawing explanation
Fig. 1 is the front view of the biological brick fuel of the present invention;
Fig. 2 is the axial sectional view of Fig. 1;
Fig. 3 is the top view of Fig. 1;
Fig. 4 is the structural representation (axially analysing and observe) of another biological carbon brick.
Detailed description of the invention
Below in conjunction with accompanying drawing, also by specific embodiment, the invention will be further described, and following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
The present invention's raw material used is commercially available, and wherein, charcoal is by organic waste, as animal wastes, and animal bone, plant roots and stems, a kind of porous carbon that wood chip and Wheat Straw etc. process.These organic wastes forming charcoal are called as " biomass ", and a lot of scientist is titled with the good reputation of charcoal " black gold ".Charcoal also can make, and method is: be made up under condition at Anaerobic Treatment 1-3 hour of stalk when temperature 500-800 DEG C.
Below be divided into three parts and discuss the present invention in detail, comprising: one, the composition of sorbing material; Two, the preparation method of sorbing material; Three, the structure of biological brick fuel made of sorbing material; Four, the preparation method of diffusion barrier in biological brick fuel; Five, the absorption example of biological brick fuel.
One, the composition of sorbing material
For water body purification sorbing material, be made up of charcoal and Sodium Polyacrylate (PAAS), the concentration of PAAS solution, at 0.1-50g/L, describedly adds 10-200g charcoal by 500-1000mLPAAS solution.The concentration of PAAS solution at 0.1-50g/L to ensure that the initial water content of sorbing material is advisable at the 60-90% of saturation moisture content.
Two, the preparation method of sorbing material
Need preparation PAAS solution according to handled waste water, PAAS solution is joined in charcoal, mixes pressing and get final product.
Three, the structure of biological brick fuel made of sorbing material
Comprise sorbing material and shell; sorbing material is filled in shell; sorbing material has exposed surface relative to shell; three metafiltration films are sealed at the exposed surface of sorbing material; described three metafiltration films are inside and outside two-layer protection filter membrane, between inside and outside two-layer protection filter membrane, arrange Pollutants Diffusion film interlayer.
The present embodiment provides a kind of concrete structure; as shown in drawings: comprise a hollow base 2; on base top, ring-type top cover 1 is installed; filling adsorption material 6 in base; the upper surface of sorbing material covers internal layer protection filter membrane 5, outer layer protection filter membrane 3; Pollutants Diffusion film interlayer 4 is set between two-layer filter membrane; the superiors' filter membrane is concordant with the upper surface of base; by the pressing of ring-type top cover; ensure fixing at chassis interior of filter membrane and sorbing material, the exposed filter membrane in the ring-type position of ring-type top cover centre is the passage of sorbing material adsorb harmful components.
The molecular weight transit dose of described diffusion barrier is 50-1000000, the aperture of outer layer protection filter membrane is 0.15-0.22 μm, internal layer protection filter sizes 0.3-0.45 μm.The thickness of described diffusion barrier is 0.8mm, and the thickness of inside and outside layer protection filter membrane is 0.1mm.
Four, the preparation method of diffusion barrier in biological brick fuel
Described diffusion barrier is by acrylamide, crosslinking agent, ammonium persulfate, N, N, the hydrogel that-methylene-bisacrylamide is made; In 100ml, weight ratio is acrylamide: crosslinking agent: ammonium persulfate: N, N ,-methylene-bisacrylamide=20:0.3:0.0035:0.2.
Its preparation method is: the crosslinking agent of the acrylamide solution of 50mL30-50wt%, 10mL1-3wt%, 40mL high purity water are mixed, add 70 μ L5-15wt% ammonium persulfates, 20 μ LN successively, N ,-methylene-bisacrylamide, pour into after mixing in mould, preparing aquagel membrane is diffusion barrier.
The molecular weight transit dose of the gel mould prepared is 50-1000000, and thickness is 0.8mm.
The preparation method of crosslinking agent is: in the 10-20mL allyl glycidyl ether added by 200-400mg sodium borohydride, obtain solution A; 5-15g agarose is added in 300mL0.3-0.5mol/LNaOH solution, constantly stir and form agarose suspension B; Solution A is added in suspension B and form solution C, solution C is stirred 12h continuously; Mixed liquor is filtered, is washed till neutrality with distilled water; Dehydration, vacuum drying, obtains required crosslinking agent.
Described sodium borohydride: allyl glycidyl ether: agarose: NaOH weight ratio=0.2-0.4:9-20:5-15:3.6-6.
Five, the absorption example of biological brick fuel
(1) be mixed with the PAAS solution of 1g/L, 100mLPAAS solution is added in 1g charcoal, charcoal is mixed with PAAS solution;
(2) mixed liquor is poured in the effigurate mould of tool, take out brick fuel;
(3) on brick fuel, cover 0.45 μm of filter membrane, diffusion barrier, 0.22 μm of filter membrane successively, and fix with support, be prepared into biological brick fuel; Diffusion barrier is diffusion barrier prepared by step 4;
(4) biological brick fuel is put into the Pb2+ solution of 500mL200mg/L, after 24h, in solution, Pb2+ concentration does not detect for dropping to.
Claims (7)
1. a biological brick fuel, it is characterized in that: comprise sorbing material and shell, sorbing material is filled in shell, sorbing material has exposed surface relative to shell, three metafiltration films are sealed at the exposed surface of sorbing material, described three metafiltration films are inside and outside two-layer protection filter membrane, between inside and outside two-layer protection filter membrane, arrange Pollutants Diffusion film interlayer;
The solution that described material is formed by charcoal and Sodium Polyacrylate, the concentration of described PAAS is at 0.1-50g/L, and the content of described charcoal is 20-400g/L.
2. biological brick fuel according to claim 1; it is characterized in that: the concrete structure of described biological brick fuel is: comprise a hollow base; on base top, ring-type top cover is coaxially installed; filling adsorption material in base; the upper surface of sorbing material covers inside and outside two-layer protection filter membrane, arranges Pollutants Diffusion film interlayer between two-layer filter membrane.
3. biological brick fuel according to claim 1, is characterized in that: it is 0.15-0.22 μm through the molecular weight 50-1000000 of material, the aperture of outer layer protection filter membrane that described diffusion barrier allows free, internal layer protection filter sizes 0.3-0.45 μm.
4. biological brick fuel according to claim 1, is characterized in that: the thickness of described diffusion barrier is 0.8mm, and the thickness of inside and outside layer protection filter membrane is 0.1mm.
5. biological brick fuel according to claim 1, it is characterized in that: the preparation method of described diffusion barrier is: acrylamide solution, crosslinking agent, high purity water are mixed, add ammonium persulfate, N successively, N,-methylene-bisacrylamide, pour into after mixing in mould, acquisition aquagel membrane is diffusion barrier.
6. biological brick fuel according to claim 5, is characterized in that: the preparation method of described crosslinking agent is: in the allyl glycidyl ether added by sodium borohydride, obtain solution A; Agarose is added in NaOH solution, constantly stir and form agarose suspension B; Solution A is added in suspension B and form solution C, solution C is stirred 12h continuously; Mixed liquor is filtered, is washed till neutrality with distilled water; Dehydration, vacuum drying, obtains required crosslinking agent, described sodium borohydride: allyl glycidyl ether: agarose: NaOH weight ratio=0.2-0.4:9-20:5-15:3.6-6.
7. biological brick fuel according to claim 1, is characterized in that: described diffusion barrier is by acrylamide, crosslinking agent, ammonium persulfate, N, N, the hydrogel that-methylene-bisacrylamide is made.
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| CN201410008599.3A CN103752285B (en) | 2014-01-08 | 2014-01-08 | Absorbent material for water body purification and biological carbon brick |
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| CN201410008599.3A CN103752285B (en) | 2014-01-08 | 2014-01-08 | Absorbent material for water body purification and biological carbon brick |
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| CN112774633A (en) * | 2021-01-15 | 2021-05-11 | 复旦大学 | Method for preparing biochar from wet garbage and application of biochar |
| CN115286454B (en) * | 2022-08-22 | 2023-10-13 | 四川络布新材料科技有限公司 | Special fertilizer for promoting crop yield increase and preparation method thereof |
| CN116375301B (en) * | 2023-06-05 | 2023-08-18 | 山东国宏生物科技有限公司 | Soybean oil wastewater treatment method |
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| JP2002253960A (en) * | 2001-02-27 | 2002-09-10 | Tanimoto Daiki | Deodorant and production method therefor |
| CN101234341A (en) * | 2008-02-28 | 2008-08-06 | 上海交通大学 | Method for preparing functional polymer-active carbon composite material for water treatment |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150603 |