CN102921391A - Preparation method of adsorbent for effectively reducing phenol content in cigarette smoke - Google Patents
Preparation method of adsorbent for effectively reducing phenol content in cigarette smoke Download PDFInfo
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- CN102921391A CN102921391A CN2012104718055A CN201210471805A CN102921391A CN 102921391 A CN102921391 A CN 102921391A CN 2012104718055 A CN2012104718055 A CN 2012104718055A CN 201210471805 A CN201210471805 A CN 201210471805A CN 102921391 A CN102921391 A CN 102921391A
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- Prior art keywords
- phenol
- adsorbent
- preparation
- cigarette smoke
- decrease rate
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000003463 adsorbent Substances 0.000 title claims abstract description 24
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 17
- 239000000779 smoke Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229920000642 polymer Polymers 0.000 claims abstract description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 9
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 9
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 9
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical class C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 230000009514 concussion Effects 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 6
- 238000012662 bulk polymerization Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000011206 ternary composite Substances 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 description 8
- 239000002253 acid Substances 0.000 description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 239000003546 flue gas Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000011218 binary composite Substances 0.000 description 2
- 239000013068 control sample Substances 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000004868 gas analysis Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 229920000344 molecularly imprinted polymer Polymers 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000009870 specific binding Effects 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- QPVRKFOKCKORDP-UHFFFAOYSA-N 1,3-dimethylcyclohexa-2,4-dien-1-ol Chemical compound CC1=CC(C)(O)CC=C1 QPVRKFOKCKORDP-UHFFFAOYSA-N 0.000 description 1
- 150000005208 1,4-dihydroxybenzenes Chemical class 0.000 description 1
- KUFFULVDNCHOFZ-UHFFFAOYSA-N 2,4-xylenol Chemical compound CC1=CC=C(O)C(C)=C1 KUFFULVDNCHOFZ-UHFFFAOYSA-N 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 230000009871 nonspecific binding Effects 0.000 description 1
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of an adsorbent for effectively reducing the content of phenol in cigarette smoke. The phenol imprinted polymer is prepared by a mass polymerization method by utilizing a molecular imprinting technology, and the obtained adsorbent has loose and porous surface and contains a large number of holes with structures and shapes matched with phenol molecules, so that the phenol imprinted polymer has high selectivity. The adsorbent is added into the ternary composite filter tip, and the addition amount of the adsorbent can be adjusted randomly according to requirements. When the amount of the phenol added was 10 mg/liter, the decrease rate of phenol was 17.8% and the decrease rate of selectivity to tar was 11.8% as compared with the control, and when the amount of the phenol added was 20 mg/liter, the decrease rate of phenol was 28.7% and the decrease rate of selectivity to tar was 12.3% as compared with the control. The method is simple to operate, low in cost and convenient for large-scale industrial production.
Description
Technical field
The invention belongs to the cigarette material preparing technical field, be specifically related to a kind of preparation method that can effectively reduce the adsorbent of phenol content in the cigarette smoke.
Background technology
Contain the multiple harmful components such as carbon monoxide, phenol, nicotine in the flue gas that produces during cigarette burning, wherein phenol directly enters in the flue gas when cigarette burning, produce bad smell, be unfavorable for simultaneously health, therefore, effectively reduce in the cigarette smoke content of phenol significant.
Existing about reducing the record of phenol processes in the cigarette smoke in the prior art, but utilize molecular imprinting, adopt bulk polymerization to prepare the phenol imprinted polymer, and it is added in the composite tip stick not yet see report as Adsorption of Phenol agent in the cigarette smoke.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of preparation method that can effectively reduce the adsorbent of phenol content in the cigarette smoke is provided.
Purpose of the present invention is achieved by the following technical programs.
Except as otherwise noted, the percentage that adopts among the present invention is mass percent.
The preparation method of the adsorbent of phenol content in a kind of effective reduction cigarette smoke may further comprise the steps:
(1) gets the raw materials ready: accurately measure phenol 93.8 mg, 2 vinylpyridines, 0.42 mL, ethylene glycol dimethacrylate 5.7 mL, 28 mg are for subsequent use for azodiisobutyronitrile; Wherein, phenol is that microsphere, 2 vinylpyridines (2-VP) are function monomer, and ethylene glycol dimethacrylate (EDMA) is crosslinking agent, and azodiisobutyronitrile (AIBN) is initator;
(2) molecular engram: phenol is put into the 10mL chloroform dissolve fully, under 25 ℃ of conditions, shake 3h after adding 2 vinylpyridines, concussion condition 150 r/min, then add ethylene glycol dimethacrylate and azodiisobutyronitrile stirs, logical nitrogen 5 min, vacuum seal, vibration 24 h make it polymerization reaction take place in 60 ℃ water bath with thermostatic control;
(3) extraction: the polymer that step (2) obtains is pulverized, grinds, excessively put into soxhlet's extractor behind 120 mesh sieves, be that the methanol solution of 10% acetic acid is eluted to ultraviolet and detects phenol without characteristic absorption with containing volume fraction, ultraviolet detects wavelength 272 nm, then removes remaining acetic acid and methyl alcohol with alcohol immersion;
(4) drying: the polymer after the extraction places 60 ℃ of lower vacuum drying 12 h of temperature namely to get required adsorbent.
Compared with prior art, the present invention has following beneficial effect:
1, the present invention adopts polymerisation in bulk molecular engram method to prepare the polymer absorbant that the Pyrogentisinic Acid has high selectivity first, and the method is simple to operate, and is with low cost, is convenient to large-scale industrial production.
2, the adsorbent surface that obtains under the preparation method of the present invention is loose porous, and contains the hole that a large amount of structures, shape and phenol molecule are complementary, thereby the Pyrogentisinic Acid has high selectivity.
3, the adsorbent that obtains of preparation method of the present invention has higher trace effect and specific recognition, also has selectively preferably with respect to other aldehydes matters, and it has the advantages that to be easy to adsorb.
4, the adsorbent that the present invention is prepared adds in the tri compound mouth rod in varing proportions, when addition is that 10 mg/ are when propping up, compare in the same old way, the reduced rate of phenol is 17.8%, relatively the elective reduction rate of tar is 11.8%, when addition is 20 mg/ when propping up, compares in the same old way, the reduced rate of phenol is 28.7%, and the elective reduction rate of tar is 12.3% relatively.
The specific embodiment
The present invention is described in further detail below by embodiment; but be to be understood that; embodiment only is explanation of the invention; and limit the invention never in any form; various changes or modification that those skilled in the art's spirit according to the present invention is done fall within protection scope of the present invention equally.
Embodiment 1
Selection phenol is that microsphere, 2 vinylpyridines (2-VP) are function monomer, and ethylene glycol dimethacrylate (EDMA) is crosslinking agent, and azodiisobutyronitrile (AIBN) is initator; Accurately take by weighing 0.0941g phenol and be dissolved in the 10 mL chloroforms, add 2-VP 0.42 mL, and 25 ℃ of concussion 3 h (150 r/min), add again EDMA 5.7 mL, AIBN 28 mg, logical nitrogen 5 min, tube sealing under the vacuum is at 60 ℃ of waters bath with thermostatic control, 24 h that vibrate.After polymerisation is finished, through pulverizing, grinding, cross 120 order sub-sieves.The polymer that obtains is placed in the apparatus,Soxhlet's, is eluted to ultraviolet with the methanol solution that contains 10 % (v/v) acetic acid and detects phenol without characteristic absorption (detecting wavelength is 272 nm), remove remaining acetic acid and methyl alcohol with alcohol immersion again.Be placed on interior 60 ℃ of drying 12 h of vacuum drying chamber after being disposed and namely get adsorbent.(representing with MIP).
Repeat above-mentioned preparation method, following difference is arranged: do not add phenol during preparation, the adsorbent that obtains is organized adsorbent (representing with NIP) in contrast.
Test the equilibrium adsorption capacity of the adsorbent that 1 the present invention prepares
The adsorbent MIP Pyrogentisinic Acid's that method mensuration the present invention of employing equilibrium adsorption experiment prepares adsorption capacity Q.
The adsorption site of imprinted material can be divided into specific binding site and nonspecific binding site two classes.The trace effect can be used trace factor-alpha (α=Q
MIP/ Q
NIP) characterize.The trace factor is greater than 1, and showing has the trace effect.The trace factor is larger, shows that the specific binding site proportion is more, and the trace effect is better, the results are shown in Table 1.
Table 1 adsorption capacity (Q) and the trace factor (α)
As can be seen from Table 1, the adsorbent that the present invention prepares has higher trace effect and specific recognition, and the trace factor reaches 1.4426.
Test the selective of adsorbent Pyrogentisinic Acid that 2 the present invention prepare
Measured respectively MIP at phenol, hydroquinones, resorcinol, paracresol, 3, in the mixed solution of 5-xylenol and 2,4-xylenol to the adsorption capacity of each component.To select the factor (β=α
i/ α
j, i and j are respectively template molecule and non-template molecule) and expression polymer selective.Select the factor greater than 1, show that the polymer Pyrogentisinic Acid is selective.Select the factor larger, selectively better.The results are shown in Table 2.
Table 2 adsorption capacity (Q) and the trace factor (α)
By in the table 2 as can be known, the MIP Pyrogentisinic Acid has selective preferably.
Test the interpolation experiment of adsorbent in binary composite tip stick that 3 the present invention prepare
The addition that props up with 10 mg/ has carried out the contrast experiment, three samples have been prepared altogether, additive is respectively: 1. additive-free (blank cigarette, control sample) 2. 3. non-template molecularly imprinted polymer (NIP) of template molecule imprinted polymer (MIP), to its detection of carrying out tar and phenol content in the cigarette smoke, the result is as shown in table 3:
Table 3 10 mg/ prop up the flue gas analysis result of addition
Test the interpolation experiment of adsorbent in binary composite tip stick that 4 the present invention prepare
The addition that props up with 20 mg/ has carried out the contrast experiment, three samples have been prepared altogether, additive is respectively: 1. additive-free (blank cigarette, control sample) 2. 3. non-template molecularly imprinted polymer (NIP) of template molecule imprinted polymer (MIP), to its detection of carrying out tar and phenol content in the cigarette smoke, the result is as shown in table 4:
Table 4 20 mg/ prop up the flue gas analysis result of addition
Claims (1)
1. preparation method who effectively reduces the adsorbent of phenol content in the cigarette smoke may further comprise the steps:
(1) gets the raw materials ready: accurately measure phenol 93.8 mg, 2 vinylpyridines, 0.42 mL, ethylene glycol dimethacrylate 5.7 mL, 28 mg are for subsequent use for azodiisobutyronitrile;
(2) molecular engram: phenol is put into the 10mL chloroform dissolve fully, under 25 ℃ of conditions, shake 3h after adding 2 vinylpyridines, concussion condition 150 r/min, then add ethylene glycol dimethacrylate and azodiisobutyronitrile stirs, logical nitrogen 5 min, vacuum seal, vibration 24 h make it polymerization reaction take place in 60 ℃ water bath with thermostatic control;
(3) extraction: the polymer that step (2) obtains is pulverized, grinds, excessively put into soxhlet's extractor behind 120 mesh sieves, be that the methanol solution of 10% acetic acid is eluted to ultraviolet and detects phenol without characteristic absorption with containing volume fraction, ultraviolet detects wavelength 272 nm, then removes remaining acetic acid and methyl alcohol with alcohol immersion;
(4) drying: the polymer after the extraction places 60 ℃ of lower vacuum drying 12 h of temperature namely to get required adsorbent.
Priority Applications (1)
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CN2012104718055A CN102921391A (en) | 2012-11-20 | 2012-11-20 | Preparation method of adsorbent for effectively reducing phenol content in cigarette smoke |
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CN2012104718055A CN102921391A (en) | 2012-11-20 | 2012-11-20 | Preparation method of adsorbent for effectively reducing phenol content in cigarette smoke |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104788713A (en) * | 2015-03-27 | 2015-07-22 | 江苏大学 | Preparation method and application of phenol molecular imprinting doped membrane |
CN107983390A (en) * | 2017-12-08 | 2018-05-04 | 吉林师范大学 | A kind of surface imprinted carbonitride/composite titania material photocatalysis membrana and preparation method and purposes |
CN111855768A (en) * | 2020-05-13 | 2020-10-30 | 莆田学院 | Preparation method of phenol molecular imprinting sensor |
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US6852818B1 (en) * | 1999-10-23 | 2005-02-08 | Cranfield University | Molecularly imprinted polymers produced by template polymerization |
CN101613432A (en) * | 2008-06-23 | 2009-12-30 | 中国科学院生态环境研究中心 | A kind of molecular blotting polymer microsphere that is used for phenol and its production and application |
CN102702429A (en) * | 2012-06-19 | 2012-10-03 | 苏州市汉微环保科技有限公司 | Method for preparing bisphenol A molecularly imprinted polymer |
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2012
- 2012-11-20 CN CN2012104718055A patent/CN102921391A/en active Pending
Patent Citations (3)
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US6852818B1 (en) * | 1999-10-23 | 2005-02-08 | Cranfield University | Molecularly imprinted polymers produced by template polymerization |
CN101613432A (en) * | 2008-06-23 | 2009-12-30 | 中国科学院生态环境研究中心 | A kind of molecular blotting polymer microsphere that is used for phenol and its production and application |
CN102702429A (en) * | 2012-06-19 | 2012-10-03 | 苏州市汉微环保科技有限公司 | Method for preparing bisphenol A molecularly imprinted polymer |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104788713A (en) * | 2015-03-27 | 2015-07-22 | 江苏大学 | Preparation method and application of phenol molecular imprinting doped membrane |
CN104788713B (en) * | 2015-03-27 | 2018-01-16 | 江苏大学 | A kind of preparation method and applications of phenol molecular engram doping |
CN107983390A (en) * | 2017-12-08 | 2018-05-04 | 吉林师范大学 | A kind of surface imprinted carbonitride/composite titania material photocatalysis membrana and preparation method and purposes |
CN111855768A (en) * | 2020-05-13 | 2020-10-30 | 莆田学院 | Preparation method of phenol molecular imprinting sensor |
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Application publication date: 20130213 |