CN108499587A - Ag/g-C3N4The preparation of composite visible light catalyst - Google Patents
Ag/g-C3N4The preparation of composite visible light catalyst Download PDFInfo
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- CN108499587A CN108499587A CN201710105010.5A CN201710105010A CN108499587A CN 108499587 A CN108499587 A CN 108499587A CN 201710105010 A CN201710105010 A CN 201710105010A CN 108499587 A CN108499587 A CN 108499587A
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- visible light
- light catalyst
- composite visible
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 239000003054 catalyst Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 235000019441 ethanol Nutrition 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 11
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 3
- 238000010792 warming Methods 0.000 claims abstract description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 6
- 229940043267 rhodamine b Drugs 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 229920000877 Melamine resin Polymers 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 22
- 229910052709 silver Inorganic materials 0.000 description 17
- 238000005406 washing Methods 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 7
- 239000011941 photocatalyst Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 239000000975 dye Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000446313 Lamella Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/08—Nanoparticles or nanotubes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The present invention relates to a kind of Ag/g C3N4The preparation method of composite visible light catalyst.Its step is：(1) with melamine for g C3N4Raw material, be put into crucible, 550 DEG C be warming up to the rate of 10 DEG C/min in Muffle furnace, 4h, cooled to room temperature is kept to obtain faint yellow solid.(2) a certain amount of g C are weighed3N4, a certain amount of ethyl alcohol or ethylene glycol solvent is added, stirs, ultrasonic 30min.(3) 0.02~0.06mol/L AgNO are added dropwise3Solution stirs 30min.(4) above-mentioned solution is poured into reaction kettle, 110~140 DEG C of 3~5h of heating are cooled to room temperature, are washed with deionized water and absolute ethyl alcohol, and drying grinding obtains ash gray Ag/g C3N4Composite visible light catalyst.The visible light catalyst that the present invention obtains there is stronger visible light photocatalytic degradation activity, the simple easy-regulating of the catalyst preparation process, raw material to be easy to get rhodamine B, and production cost is low.
Description
Technical field
The present invention relates to a kind of Ag/g-C with visible light activity3N4The preparation of composite visible light catalyst.Belong to light to urge
Change technical field.
Background technology
With the fast development of industrial technology, environmental pollution has become the serious problems for threatening human survival and future development
One of.The application of photocatalysis technology is considered as solving a kind of effective way of water body and air pollution problems inherent.g-C3N4As one
The novel visible light responsive photocatalyst of kind, has unique electronic structure, relatively narrow energy gap and suitable position of energy band,
And there is higher thermal stability and chemical stability, but it is relatively narrow to the response range of visible light, therefore, prepares with visible
The high efficiency photocatalyst of photoresponse is an important topic of current photocatalysis research field.
By solvent-thermal method in g-C3N4Supported on carriers Ag nano particles are to expand g-C3N4One kind of visible light-responded range
Effective way.Since plasma resonance absorption existing for Ag nano particles acts on, can widen composite photo-catalyst significantly can
Light-exposed response, and the separative efficiency of photo-generated carrier is significantly improved, and then effectively improve its photocatalytic activity, therefore, nanometer Ag
Particle can be used for expanding g-C3N4It is visible light-responded.The present invention by a kind of simple solvent-thermal method, by Ag nano particles with
g-C3N4Stratified material is compound, prepared different quality than Ag/g-C3N4Composite visible light catalyst makes its absorption spectrum
It is expanded to visible light region, to improve photocatalysis efficiency.
Silver nitrate solution is added drop-wise in dicyanodiamine or melamine dispersion liquid by patent application CN 104475140A, will be obtained
Product be put into high-temperature atmosphere furnace, obtain Ag/g-C in nitrogen protection3N4Composite photo-catalyst, under visible light illumination to organic
Dye, rhodamine B has preferable photocatalytic degradation effect.But the Ag grain diameters that the method obtains are larger, and preparation process is more multiple
It is miscellaneous.This patent is with the g-C of stratiform3N4For carrier, Ag nano particles are load, pass through a step solvent structure not homogeneity
Measure the Ag/g-C of ratio3N4Composite visible light catalyst, Ag nano particles uniform load is in g-C3N4On lamella carrier, nanometer is utilized
The unique plasma resonance effect of silver has widened the visible light-responded range of composite photo-catalyst, improves its photocatalysis performance,
Show efficient visible light photocatalytic degradation rhodamine B activity.
Invention content
In order to solve the above problem, used technical solution is the present invention：Solvent-thermal method prepare different quality than Ag/g-
C3N4Composite photo-catalyst, according to the content of claims, it is characterised in that include the following steps：
(1) it is g-C with melamine3N4Raw material, be put into crucible, be warming up to the rate of 10 DEG C/min in Muffle furnace
550 DEG C, 4h, cooled to room temperature is kept to obtain faint yellow solid；
(2) a certain amount of g-C is weighed3N4, 60~80mL solvents are added, solvent is ethyl alcohol or ethylene glycol, stirring, ultrasonic 30min
It is made to be uniformly dispersed；
(3) g-C is stirred on side3N40.02~0.06mol/L AgNO are added dropwise in solution side3Solution stirs 30min；
(4) solution being stirred is poured into reaction kettle, 110~140 DEG C of 3~5h of heating are cooled to room temperature, with deionized water and
Absolute ethyl alcohol washs, and dries, grinding.Obtain ash gray Ag/g-C3N4Composite visible light catalyst.
By said program, the solvent described in step (2) includes ethyl alcohol and ethylene glycol, and addition is 60~80mL.
By said program, the AgNO described in step (3)3Solution concentration is 0.02~0.06mol/L, m (Ag)/m (g-C3N4) it is 5
~30.
By said program, heating temperature is 110~140 DEG C in step (4) described reaction kettle, and heating time is 3~5h.
Using dye, rhodamine B as probe molecule, prepared Ag/g-C is evaluated3N4Composite photo-catalyst is under visible light illumination
Photocatalytic activity.It weighs 0.1g catalyst samples and 100mL is added, in the RB aqueous solutions of 0.01g/L, ultrasonic 10min is carried out dark
30min is reacted, light source uses 500W xenon lamps, it is seen that gloss is obtained with the optical filter that cutoff wavelength is 400nm, light intensity 12mW/
cm2.It is 15cm that liquid level spacing in light source and beaker is kept in reaction, is sampled every 10min, and reaction suspension centrifuges, on
752 type ultraviolet-uisible spectrophotometers of layer clear liquid measure absorbance values of the RB at 554nm, are drawn by Lambert-Beer's law
Go out relative concentration versus time curve C/Co~t.
Advantages of the present invention：G-C is prepared with simple thermal polymerization3N4As carrier, by a step alcohol solvent thermal reduction
Novel Ag/g-C is synthesized3N4Composite visible light catalyst, under visible light being capable of effective rhodamine B degradation dyestuff.Nanometer Ag
Particulate load is in g-C3N4On lamella carrier, visible absorption range has been widened, has improved the photocatalysis performance of composite catalyst,
And it is evaluated through multiple loop test functional.The simple easy-regulating of preparation process, production cost is low, is suitable for mass production.
Description of the drawings
Fig. 1 prepares Ag/g-C3N4The process flow chart of composite visible light catalyst.
Fig. 2A g/g-C3N4The TEM photos of composite visible light catalyst,
Fig. 3 Ag/g-C3N4Curve graph of the composite visible light catalyst to rhodamine B photocatalytic degradation.
Specific implementation mode
The present invention is described in further details with reference to embodiment, but protection scope of the present invention is not limited to these realities
Apply example.
Embodiment 1
5%Ag/g-C3N4
(1) g-C of 1g is weighed3N4It is added in the alcohol solvent of 50mL；Ultrasonic 30min.
(2) AgNO of 0.045mol/L is added dropwise dropwise3Solution 10mL stirs 30min；
(3) solution prepared is poured into reaction kettle, 120 DEG C of heating 3h are cooled to room temperature, with deionized water and absolute ethyl alcohol
Washing is dried, grinding.Obtain ash gray 5%Ag/g-C3N4Composite visible light catalyst.
Embodiment 2
10%Ag/g-C3N4
(1) g-C of 1g is weighed3N4It is added in the alcohol solvent of 50mL；Ultrasonic 30min.
(2) AgNO of 0.045mol/L is added dropwise dropwise3Solution 20mL stirs 30min；
(3) solution prepared is poured into reaction kettle, 120 DEG C of heating 3h are cooled to room temperature, with deionized water and absolute ethyl alcohol
Washing is dried, grinding.Obtain ash gray 10%Ag/g-C3N4Composite visible light catalyst.
Embodiment 3
15%Ag/g-C3N4
(1) g-C of 1g is weighed3N4It is added in the alcohol solvent of 50mL；Ultrasonic 30min.
(2) AgNO of 0.045mol/L is added dropwise dropwise3Solution 30mL stirs 30min；
(3) solution prepared is poured into reaction kettle, 120 DEG C of heating 3h are cooled to room temperature, with deionized water and absolute ethyl alcohol
Washing is dried, grinding.Obtain ash gray 15%Ag/g-C3N4Composite visible light catalyst.
20%Ag/g-C3N4
(1) g-C of 1g is weighed3N4It is added in the alcohol solvent of 50mL；Ultrasonic 30min.
(2) AgNO of 0.045mol/L is added dropwise dropwise3Solution 40mL stirs 30min；
(3) solution prepared is poured into reaction kettle, 120 DEG C of heating 3h are cooled to room temperature, with deionized water and absolute ethyl alcohol
Washing is dried, grinding.Obtain ash gray 20%Ag/g-C3N4Composite visible light catalyst.
Embodiment 5
25%Ag/g-C3N4
(1) g-C of 1g is weighed3N4It is added in the alcohol solvent of 50mL；Ultrasonic 30min.
(2) AgNO of 0.045mol/L is added dropwise dropwise3Solution 50mL stirs 30min；
(3) solution prepared is poured into reaction kettle, 120 DEG C of heating 3h are cooled to room temperature, with deionized water and absolute ethyl alcohol
Washing is dried, grinding.Obtain ash gray 25%Ag/g-C3N4Composite visible light catalyst.
Embodiment 6
30%Ag/g-C3N4
(1) g-C of 1g is weighed3N4It is added in the alcohol solvent of 50mL；Ultrasonic 30min.
(2) AgNO of 0.045mol/L is added dropwise dropwise3Solution 60mL stirs 30min；
(3) solution prepared is poured into reaction kettle, 120 DEG C of heating 3h are cooled to room temperature, with deionized water and absolute ethyl alcohol
Washing is dried, grinding.Obtain ash gray 5%Ag/g-C3N4Composite visible light catalyst.
Embodiment 7
The 25%Ag/g-C that heating temperature is 140 DEG C3N4
(1) g-C of 1g is weighed3N4It is added in the alcohol solvent of 50mL；Ultrasonic 30min.
(2) AgNO of 0.045mol/L is added dropwise dropwise3Solution 50mL stirs 30min；
(3) solution prepared is poured into reaction kettle, 140 DEG C of heating 3h are cooled to room temperature, with deionized water and absolute ethyl alcohol
Washing is dried, grinding.Obtain ash gray 25%Ag/g-C3N4Composite visible light catalyst.
Embodiment 7
Heating time is the 25%Ag/g-C of 5h3N4
(1) g-C of 1g is weighed3N4It is added in the alcohol solvent of 50mL；Ultrasonic 30min.
(2) AgNO of 0.045mol/L is added dropwise dropwise3Solution 50mL stirs 30min；
(3) solution prepared is poured into reaction kettle, 120 DEG C of heating 5h are cooled to room temperature, with deionized water and absolute ethyl alcohol
Washing is dried, grinding.Obtain ash gray 25%Ag/g-C3N4Composite visible light catalyst.
Claims (6)
1.Ag/g-C3N4The preparation of composite visible light catalyst, it is characterised in that with sheet g-C3N4For carrier, nanometer Ag is negative
Supporting agent includes the following steps：
(1) it is g-C with melamine3N4Raw material, be put into crucible, 550 be warming up to the rate of 10 DEG C/min in Muffle furnace
DEG C, keep 4h, cooled to room temperature to obtain faint yellow solid；
(2) a certain amount of g-C is weighed3N4, the solvent of 60~80mL is added, solvent is ethyl alcohol or ethylene glycol, stirring, ultrasonic 30min
It is made to be uniformly dispersed；
(3) g-C is stirred on side3N40.02~0.06mol/L AgNO are added dropwise in solution side3Solution stirs 30min；
(4) solution being stirred is poured into reaction kettle, 110~140 DEG C of 3~5h of heating are cooled to room temperature, with deionized water and
Absolute ethyl alcohol washs, and dries, grinding.Obtain ash gray Ag/g-C3N4Composite visible light catalyst.
2. according to the Ag/g-C described in right 13N4The preparation of composite visible light catalyst, it is characterised in that：Solvent include ethyl alcohol,
Ethylene glycol, addition are 60~80mL.
3. according to the Ag/g-C described in right 13N4The preparation of composite visible light catalyst, it is characterised in that：AgNO is added dropwise3Solution
A concentration of 0.02~0.06mol/L.
4. according to the Ag/g-C described in right 13N4The preparation of composite visible light catalyst, it is characterised in that：m(Ag)/m(g-C3N4)
It is 5~30.
5. according to the Ag/g-C described in right 13N4The preparation of composite visible light catalyst, it is characterised in that：It heats in a kettle
Temperature be 110~140 DEG C.
6. according to the Ag/g-C described in right 13N4The preparation of composite visible light catalyst, it is characterised in that：It heats in a kettle
Time is 3~5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710105010.5A CN108499587A (en) | 2017-02-25 | 2017-02-25 | Ag/g-C3N4The preparation of composite visible light catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710105010.5A CN108499587A (en) | 2017-02-25 | 2017-02-25 | Ag/g-C3N4The preparation of composite visible light catalyst |
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| Publication Number | Publication Date |
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| CN108499587A true CN108499587A (en) | 2018-09-07 |
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ID=63373560
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| CN201710105010.5A Pending CN108499587A (en) | 2017-02-25 | 2017-02-25 | Ag/g-C3N4The preparation of composite visible light catalyst |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110787828A (en) * | 2019-10-23 | 2020-02-14 | 西北工业大学 | AgNWs/g-C3N4Preparation method of photodegradation catalyst |
| CN112442707A (en) * | 2020-11-30 | 2021-03-05 | 哈尔滨理工大学 | Flaky high-catalytic-activity g-C3N4Method for preparing powder |
| CN113559906A (en) * | 2021-07-21 | 2021-10-29 | 南京工大环境科技南通有限公司 | Method for preparing semiconductor coupling composite photocatalyst for treating refractory wastewater |
| CN113731410A (en) * | 2021-09-24 | 2021-12-03 | 太原理工大学 | Ag2V4O11/g-C3N4Preparation method and application of composite photocatalyst |
| CN114360922A (en) * | 2022-01-17 | 2022-04-15 | 南京信息工程大学 | Ag/g-C3N4Composite material and electrode material prepared from same |
-
2017
- 2017-02-25 CN CN201710105010.5A patent/CN108499587A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110787828A (en) * | 2019-10-23 | 2020-02-14 | 西北工业大学 | AgNWs/g-C3N4Preparation method of photodegradation catalyst |
| CN110787828B (en) * | 2019-10-23 | 2022-12-06 | 西北工业大学 | AgNWs/g-C 3 N 4 Preparation method of photodegradation catalyst |
| CN112442707A (en) * | 2020-11-30 | 2021-03-05 | 哈尔滨理工大学 | Flaky high-catalytic-activity g-C3N4Method for preparing powder |
| CN113559906A (en) * | 2021-07-21 | 2021-10-29 | 南京工大环境科技南通有限公司 | Method for preparing semiconductor coupling composite photocatalyst for treating refractory wastewater |
| CN113731410A (en) * | 2021-09-24 | 2021-12-03 | 太原理工大学 | Ag2V4O11/g-C3N4Preparation method and application of composite photocatalyst |
| CN113731410B (en) * | 2021-09-24 | 2024-03-15 | 太原理工大学 | Ag (silver) alloy 2 V 4 O 11 /g-C 3 N 4 Preparation method and application of composite photocatalyst |
| CN114360922A (en) * | 2022-01-17 | 2022-04-15 | 南京信息工程大学 | Ag/g-C3N4Composite material and electrode material prepared from same |
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180907 |