CN103071498A - Preparation method of Cu2O compound photocatalyst - Google Patents
Preparation method of Cu2O compound photocatalyst Download PDFInfo
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- CN103071498A CN103071498A CN2013100124705A CN201310012470A CN103071498A CN 103071498 A CN103071498 A CN 103071498A CN 2013100124705 A CN2013100124705 A CN 2013100124705A CN 201310012470 A CN201310012470 A CN 201310012470A CN 103071498 A CN103071498 A CN 103071498A
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- ethyl alcohol
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- expanded graphite
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- -1 Cu2O compound Chemical class 0.000 title abstract description 4
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title abstract 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 26
- 239000010439 graphite Substances 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 150000001879 copper Chemical class 0.000 claims abstract description 5
- 239000012266 salt solution Substances 0.000 claims abstract description 5
- 239000006228 supernatant Substances 0.000 claims abstract description 5
- 239000010949 copper Substances 0.000 claims description 27
- 239000002131 composite material Substances 0.000 claims description 20
- 238000001556 precipitation Methods 0.000 claims description 17
- 230000001699 photocatalysis Effects 0.000 claims description 10
- 238000007146 photocatalysis Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000008236 heating water Substances 0.000 claims description 4
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 3
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 239000011449 brick Substances 0.000 claims 2
- 239000010881 fly ash Substances 0.000 claims 2
- 238000000034 method Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000005749 Copper compound Substances 0.000 abstract description 4
- 150000001880 copper compounds Chemical class 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract 2
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 abstract 1
- 229910017912 NH2OH Inorganic materials 0.000 abstract 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000011010 flushing procedure Methods 0.000 abstract 1
- 231100001261 hazardous Toxicity 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 230000001473 noxious effect Effects 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 238000011160 research Methods 0.000 description 5
- 239000000356 contaminant Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000007770 graphite material Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- OEHNVKBOQOXOJN-UHFFFAOYSA-N 2-(4-nitrophenyl)phenol Chemical compound OC1=CC=CC=C1C1=CC=C([N+]([O-])=O)C=C1 OEHNVKBOQOXOJN-UHFFFAOYSA-N 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
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- Catalysts (AREA)
Abstract
The invention provides a preparation method of a Cu2O compound photocatalyst. The method includes the following steps: mixing distilled water, absolute ethyl alcohol and a copper salt solution, adding EG (expanded graphite) and evenly stirring, then adding a NaOH solution and absolute ethyl alcohol, and finally adding an NH2OH*HC1 solution, stirring and standing; heating the prepared solution in a water bath and stirring, removing the supernatant after layering after the reaction is over, flushing and precipitating; and finally dissolving the precipitating in absolute ethyl alcohol, drying to prepare the Cu2O compound photocatalyst. The method takes EG and a copper compound as the raw materials to prepare an EG-loaded nano Cu2O sample, the raw material source is easy, the cost is low, the preparation technology is simple, requirements for equipment are low, and the operability is good; and nano-particles in the prepared photocatalyst are uniformly loaded on the EG surface, and the photocatalyst can degrade hazardous and noxious substances under the condition of visible light, is simple in recycling, and is quite suitable for processing organic pollutants.
Description
Technical field
The present invention relates to the photochemical catalyst preparing technical field in the Chemical Engineering, specifically a kind of Cu
2The preparation method of O composite photocatalyst.
Background technology
In recent years, nanometer Cu
2O progressively has been subject to Environmental Studies person's attention because it has superior photocatalysis performance aspect environmental pollution improvement, be the TiO that continues
2New Generation Optical catalyst afterwards is a kind of environmental protection photochemical catalyst that has DEVELOPMENT PROSPECT.Relevant studies show that is with nanometer Cu
2O is photochemical catalyst, utilizes sunshine as the research of light source treatment of dyeing and printing, shows Cu
2O heterogeneous catalysis method may become the effective way that waste water from dyestuff is administered.
In order to improve Cu
2The photocatalysis performance of O can carry out modification to it.Relevant scholar is to Cu
2The research of the synthetic and photocatalysis performance of O internal carbon-inlaid nano pipe composite balls has illustrated Cu
2The photocatalytic activity of O composite balls p-nitrophenyl phenol solution compares Cu
2O exceeds about 10%.Yet CNT is not suitable for industrial production owing to expensive, so replace carbon nanotube loaded Cu with cheap carrier
2O just becomes researcher's research emphasis.
Expanded graphite is that native graphite obtains a kind of lamellar compound through the strong oxidizer oxidation, has the characteristics such as specific area is large, the interlayer ion exchange capacity is strong, and these characteristics are conducive to the compound of expanded graphite and inorganic material.Demonstrated many superior performances with expanded graphite as the prepared nano composite material of carrier, and its cost is more much lower than carbon nano tube compound material, thereby has potential application prospect.Present research mainly concentrates on expanded graphite/organic matter nano composite material aspect, and is relatively less about the research of expanded graphite/composite material of inorganic matter.
Based on above analysis, the present invention prepares a kind of Cu take expanded graphite and copper compound as raw material by direct precipitation method
2The O composite photocatalyst, this catalyst preparation cost is low, and preparation technology is simple, and is low for equipment requirements, and operability is good, can the efficient degradation poisonous and harmful substance under visible light, recycle simply, be highly suitable for the deep treatment of waste water from dyestuff.
Summary of the invention
The object of the present invention is to provide a kind of Cu
2The preparation method of O composite photocatalyst take expanded graphite and copper compound as raw material, prepares expanded graphite supporting nanometer Cu by direct precipitation method
2The O sample, this preparation technology is simple, and cost is low, and is low for equipment requirements, and operability is good.
Technical scheme provided by the invention is: a kind of Cu
2The preparation method of O composite photocatalyst is characterized in that comprising the steps:
(1) copper salt solution with 0.5 mol/L of the absolute ethyl alcohol of the distilled water of 83.4 unit volumes, 20 unit volumes and 5 unit volumes mixes, then adding expanded graphite stirs, then alternately add the NaOH solution of 1.0 mol/L of 9 unit volumes and the absolute ethyl alcohol of 30 unit volumes, all add at last the NH of 0.5 mol/L of 0.5 ~ 15 unit volume
2OHHCl solution left standstill after the stirring 1 ~ 6 hour;
(2) gained solution in the step 1 is carried out heating water bath also stirred in 1 ~ 30 minute, after solution reaction is finished layering, outwell supernatant liquor, mixed solution with absolute ethyl alcohol and distilled water washes precipitation, at last precipitation is dissolved in the absolute ethyl alcohol, 20 ~ 80 ℃ of lower oven dry precipitations, namely get a kind of Cu
2The O composite photocatalyst.
Copper salt solution in the described step 1 is CuCl
2Or Cu (NO
3)
2Solution, the mass ratio of mantoquita and expanded graphite are 5:1 ~ 1:1.
The load capacity of expanded graphite is 10% ~ 50% in the described step 1.
Add NH in the described step 1
2The time of OHHCl solution is 1 ~ 30 second.
Be used in the described step 2 washing in the mixed solution of precipitation, the volume ratio of absolute ethyl alcohol and distilled water is 1:1.
The invention has the beneficial effects as follows:
(1) among the present invention take expanded graphite and copper compound as raw material, prepare expanded graphite supporting nanometer Cu by direct precipitation method
2The O sample, the raw material that adopt source is easy, and price is low, and preparation technology is simple, and is low for equipment requirements, and operability is good;
(2) in the photochemical catalyst of the present invention preparation the nano particle uniform load on the expanded graphite surface, can be under the visible light condition efficient degradation poisonous and harmful substance, recycle simply, be highly suitable for the processing of organic pollution;
(3) expanded graphite has the characteristics such as specific area is large, the interlayer ion exchange capacity is strong, these characteristics are conducive to the compound of expanded graphite and inorganic material, have good synergy with expanded graphite as the prepared nano-photo catalytic composite of carrier, can greatly improve its photocatalytic degradation ability.
The specific embodiment
The present invention will be further described below in conjunction with specific embodiment, and the present invention is not limited only to these embodiment.
Embodiment 1:
A kind of Cu
2The preparation method of O composite photocatalyst is characterized in that comprising the steps:
(1) with the CuCl of 0.5 mol/L of the absolute ethyl alcohol of the distilled water of 83.4ml, 20ml and 5ml
2Solution mixes, and then adds expanded graphite and stirs, and wherein the mass ratio of mantoquita and expanded graphite is 5:1, then alternately adds the NaOH solution of 1.0 mol/L of 9ml and the absolute ethyl alcohol of 30ml, the last NH that all added 0.5 mol/L of 9.8ml in 5 seconds
2OHHCl solution left standstill after the stirring 6 hours;
(2) gained solution in the step 1 is carried out heating water bath also stirred in 10 minutes, after solution reaction is finished layering, outwell supernatant liquor, be that the absolute ethyl alcohol of 1:1 and the mixed solution of distilled water wash precipitation with volume ratio, at last precipitation is dissolved in the absolute ethyl alcohol, 75 ℃ of lower oven dry precipitations, namely get a kind of Cu
2The O composite photocatalyst.
This composite photocatalyst is carried out the photocatalytic degradation experiment according to the evaluation method of photocatalysis degradation organic contaminant, found that the degradation rate of methyl orange can reach 98%.
Embodiment 2:
A kind of Cu
2The preparation method of O composite photocatalyst is characterized in that comprising the steps:
(1) with the Cu (NO of 0.5 mol/L of the absolute ethyl alcohol of the distilled water of 83.4ml, 20ml and 5ml
3)
2Solution mixes, and then adds expanded graphite and stirs, and wherein the mass ratio of mantoquita and expanded graphite is 1:1, then alternately adds the NaOH solution of 1.0 mol/L of 9ml and the absolute ethyl alcohol of 30ml, the last NH that all added 0.5 mol/L of 15ml in 25 seconds
2OHHCl solution left standstill after the stirring 1.5 hours;
(2) gained solution in the step 1 is carried out heating water bath also stirred in 20 minutes, after solution reaction is finished layering, outwell supernatant liquor, be that the absolute ethyl alcohol of 1:1 and the mixed solution of distilled water wash precipitation with volume ratio, at last precipitation is dissolved in the absolute ethyl alcohol, 50 ℃ of lower oven dry precipitations, namely get a kind of Cu
2The O composite photocatalyst.
This composite photocatalyst is carried out the photocatalytic degradation experiment according to the evaluation method of photocatalysis degradation organic contaminant, found that the degradation rate of methyl orange can reach 93%.
The evaluation method of photocatalysis degradation organic contaminant: take methyl orange as target contaminant, the methyl orange solution of configuration 30mg/L, the catalyst sample of 100mg is added in the 90mL methyl orange solution, carries out under these conditions the catalytic decolorization degraded of methyl orange solution, in this process, continue to stir.At first dark reaction is 30 minutes, gets subsequently the 6mL sample, immediately the centrifugal photochemical catalyst of removing.With the absorbance of 722 type spectrophotometric determination clear liquids at λ max=464nm place.Afterwards, carry out light-catalyzed reaction, got one time sample every 10 minutes, survey the absorbance of materialsing, it is 2 hours that total duration is tested in photocatalysis.Obtain the ultraviolet-visible absorption spectroscopy of sample after 90 minutes.
Claims (5)
1. Cu
2The preparation method of O composite photocatalyst is characterized in that comprising the steps:
(1) copper salt solution with 0.5 mol/L of the absolute ethyl alcohol of the distilled water of 83.4 unit volumes, 20 unit volumes and 5 unit volumes mixes, then adding expanded graphite stirs, then alternately add the NaOH solution of 1.0 mol/L of 9 unit volumes and the absolute ethyl alcohol of 30 unit volumes, all add at last the NH of 0.5 mol/L of 0.5 ~ 15 unit volume
2OHHCl solution left standstill after the stirring 1 ~ 6 hour;
(2) gained solution in the step 1 is carried out heating water bath also stirred in 1 ~ 30 minute, after solution reaction is finished layering, outwell supernatant liquor, mixed solution with absolute ethyl alcohol and distilled water washes precipitation, at last precipitation is dissolved in the absolute ethyl alcohol, 20 ~ 80 ℃ of lower oven dry precipitations, namely get a kind of Cu
2The O composite photocatalyst.
2. require described a kind of Cu according to claim 1
2The preparation method of O composite photocatalyst is characterized in that: the copper salt solution in the described step 1 is CuCl
2Or Cu (NO
3)
2Solution, the mass ratio of mantoquita and expanded graphite are 5:1 ~ 1:1.
3. require described a kind of Cu according to claim 1
2The preparation method of O composite photocatalyst is characterized in that: the load capacity of expanded graphite is 10% ~ 50% in the described step 1.
4. according to the preparation method of a kind of fly ash base photocatalysis brick claimed in claim 1, it is characterized in that: add NH in the described step 1
2The time of OHHCl solution is 1 ~ 30 second.
5. according to the preparation method of a kind of fly ash base photocatalysis brick claimed in claim 1, it is characterized in that: be used in the described step 2 washing in the mixed solution of precipitation, the volume ratio of absolute ethyl alcohol and distilled water is 1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310012470.5A CN103071498B (en) | 2013-01-14 | 2013-01-14 | Preparation method of Cu2O compound photocatalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310012470.5A CN103071498B (en) | 2013-01-14 | 2013-01-14 | Preparation method of Cu2O compound photocatalyst |
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| Publication Number | Publication Date |
|---|---|
| CN103071498A true CN103071498A (en) | 2013-05-01 |
| CN103071498B CN103071498B (en) | 2015-04-22 |
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|---|---|---|---|
| CN201310012470.5A Expired - Fee Related CN103071498B (en) | 2013-01-14 | 2013-01-14 | Preparation method of Cu2O compound photocatalyst |
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|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217868A (en) * | 2017-12-07 | 2018-06-29 | 吴亚琴 | A kind of preparation method of high alga-killing rate composite algicide |
| CN110496624A (en) * | 2019-08-22 | 2019-11-26 | 四川建筑职业技术学院 | A kind of composite material and preparation method for sewage treatment |
| CN113117676A (en) * | 2021-03-08 | 2021-07-16 | 新乡学院 | Cu2Preparation method of O-CuO/bentonite photocatalytic composite material |
| CN113441156A (en) * | 2021-06-24 | 2021-09-28 | 青岛科技大学 | Hollowed-out spherical structure Cu2O/Cu9S5Photocatalytic material and preparation method and application thereof |
| CN114250627A (en) * | 2021-11-30 | 2022-03-29 | 盐城工学院 | Preparation method of cuprous oxide composite material for finishing cotton fabric |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217868A (en) * | 2017-12-07 | 2018-06-29 | 吴亚琴 | A kind of preparation method of high alga-killing rate composite algicide |
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| CN110496624A (en) * | 2019-08-22 | 2019-11-26 | 四川建筑职业技术学院 | A kind of composite material and preparation method for sewage treatment |
| CN113117676A (en) * | 2021-03-08 | 2021-07-16 | 新乡学院 | Cu2Preparation method of O-CuO/bentonite photocatalytic composite material |
| CN113441156A (en) * | 2021-06-24 | 2021-09-28 | 青岛科技大学 | Hollowed-out spherical structure Cu2O/Cu9S5Photocatalytic material and preparation method and application thereof |
| CN114250627A (en) * | 2021-11-30 | 2022-03-29 | 盐城工学院 | Preparation method of cuprous oxide composite material for finishing cotton fabric |
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| Publication number | Publication date |
|---|---|
| CN103071498B (en) | 2015-04-22 |
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Owner name: SHANXI SHUOBO TECHNOLOGY CO., LTD. Effective date: 20150505 Owner name: TAIYUAN UNIV. OF TECHNOLOGY Free format text: FORMER OWNER: DU YALI Effective date: 20150505 |
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Inventor after: Wu Xu Inventor after: Du Yali Inventor after: Zhu Baolin Inventor after: Zhao Qiang Inventor after: Song Shaofei Inventor after: Liu Youjun Inventor before: Du Yali Inventor before: Zhu Baolin Inventor before: Zhao Qiang Inventor before: Song Shaofei Inventor before: Liu Youjun |
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Free format text: CORRECT: INVENTOR; FROM: DU YALI ZHU BAOLIN ZHAO QIANG SONG SHAOFEI LIU YOUJUN TO: WU XU DU YALI ZHU BAOLIN ZHAO QIANG SONG SHAOFEI LIU YOUJUN |
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Effective date of registration: 20150505 Address after: 030024 Yingze, Shanxi Province, Berlin District, West Street, No. 79, No. Patentee after: Taiyuan University of Technology Patentee after: Shanxi Yuan Technology Co., Ltd. Address before: 030024 room 1006, science and technology building, Taiyuan University of Technology, 79 West Avenue, Wan Berlin District, Shanxi, Taiyuan, Yingze Patentee before: Du Yali |
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Granted publication date: 20150422 Termination date: 20160114 |
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| CF01 | Termination of patent right due to non-payment of annual fee |