CN103436991A - Nanofiber with specific surface area capable of being increased - Google Patents
Nanofiber with specific surface area capable of being increased Download PDFInfo
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- CN103436991A CN103436991A CN2013103817664A CN201310381766A CN103436991A CN 103436991 A CN103436991 A CN 103436991A CN 2013103817664 A CN2013103817664 A CN 2013103817664A CN 201310381766 A CN201310381766 A CN 201310381766A CN 103436991 A CN103436991 A CN 103436991A
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- nanofiber
- spinning solution
- surface area
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- specific surface
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 31
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000835 fiber Substances 0.000 claims abstract description 17
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 15
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 7
- 238000009987 spinning Methods 0.000 claims description 55
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 12
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 12
- 238000001523 electrospinning Methods 0.000 claims description 11
- 239000004745 nonwoven fabric Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 6
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 claims description 6
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 6
- 238000005421 electrostatic potential Methods 0.000 claims description 4
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 2
- 238000005253 cladding Methods 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000004020 conductor Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- SKRWFPLZQAAQSU-UHFFFAOYSA-N stibanylidynetin;hydrate Chemical compound O.[Sn].[Sb] SKRWFPLZQAAQSU-UHFFFAOYSA-N 0.000 abstract 5
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical group O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 abstract 2
- 229920000642 polymer Polymers 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 235000010215 titanium dioxide Nutrition 0.000 description 5
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229920002301 cellulose acetate Polymers 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 229920001746 electroactive polymer Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 150000002605 large molecules Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000010094 polymer processing Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Landscapes
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Multicomponent Fibers (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention relates to a nanofiber with the specific surface area capable of being increased. The high-surface-area nanofiber has a nuclear-shell structure, a nuclear layer is made of titanium dioxide (TiO2), a shell layer is made of antimony tin oxide (ATO), the antimony tin oxide in the shell layer is SnO2 doped with a Sb element, wherein the mass percentage of the Sb element is 20-80%; the fiber structure is of a nuclear-shell structure formed by the process that the titanium dioxide is coated with the antimony tin oxide, wherein the mass percentage of the TiO2 is 20-80%, the mass percentage of the ATO is 20-80%; the average diameter of the nanofiber which is of the nuclear-shell structure is 100-450nm. The nanofiber which is of the nuclear-shell structure is prepared by using an electrostatic spinning technique, the preparation method is simple and easy to implement, and according to the obtained nanofiber material, the cost of conductive materials is lowered, and the nanofiber has a great specific surface area.
Description
Technical field
But the present invention relates to a kind of nanofiber of increasing specific surface area.
Background technology
Electrostatic spinning technique is realized in 1934 by Formhals etc. the earliest.From eighties of last century eighties (before and after about nineteen ninety-five) particularly recently for over ten years, be subject to the promotion of Nano-technology Development upsurge, Static Spinning receives publicity again, utilize this technology, be easy to many Polymer Processing are become the superfine fibre of different fibre structures, different scale (sub-micron is to nanometer).
The polymer nanofiber that utilizes electrostatic spinning technique successfully to prepare comprises poly-phthalein amine (PA6, PA66), polyacrylonitrile (PAN), polyvinyl alcohol (PVA), polyethylene glycol oxide (PEO), PLA (PLA), cellulose acetate (CA), polyurethane (PU), many polymeric matrixs such as PC (PCL).Chinese patent " a kind of preparation method and application of affinity vinyl cyanide base co-polymer superfine fibre film " (publication number CNl01185851) is dissolved in acrylonitrile copolymer in solvent, carry out electrostatic spinning, prepare a kind of affinity vinyl cyanide co-polymer superfine fibre film, fibre diameter is 80-800run.United States Patent (USP) Electrospun electroactive polymers (publication number 20060057377) will be with the polymer of polar group, as polyamide, polyurethane, polyacrylic acid etc. are dissolved in solvent, carry out electrostatic spinning, prepared and had the active polymer nanofiber of conduction, fibre diameter is 10-10000nm.On utilize at present method of electrostatic spinning to prepare polymer nanofiber-based, be the polymeric matrix of normal temperature in glassy state or crystalline state, because the large molecule of these polymer is under electrostatic induction by super drawing and after ejecting fiber, can again change glassy state or crystalline state into rapidly in the quick volatilization process of solvent or in the fast cooling cooling procedure and be fixed up, fiber is indeformable, easily controls the stability of spinning process.
Titanium dioxide; be commonly called as titanium dioxide; of light color; stable in properties, have good covering power and semi-conductive performance, and valuable especially is that titanium white is nontoxic; inexpensive; raw material sources are extensive, and use cost is low, are applied to the aspects such as rubber industry, plastics industry, paper industry, coatings industry, daily use chemicals and medical industry, food industry, environmental protection more.
ATO, the Chinese name tin-antiomony oxide, have good light transmission and electric conductivity, can do good heat-insulating powder, conducting powder (antistatic powder) use, and the heat-proof quality that it is good, be widely used in the fields such as coating, chemical fibre, polymeric membrane; As conductive material, the incomparable advantage of other conductive materials (as graphite, surfactant, metal powder etc.) is arranged in dispersiveness, anti-activity, thermoplasticity, ABRASION RESISTANCE, security, be applied to the aspects such as photoelectric display device, transparency electrode, solar cell, liquid crystal display, catalysis more, but ATO is expensive, use cost is higher, and powder is navy blue, limited to a certain extent its application.
TiO
2with the preparation of ATO composite, met the requirement of material to color, reduced the cost of conductive material, improved the using value of material.And TiO
2preparation present stage research of/ATO composite is less, in the related data of finding, has adopted chemical coprecipitation method more, by TiO
2surface coats ATO and prepares conductive powder body, and the product application has certain limitation.
Summary of the invention
But the present invention has designed a kind of nanofiber of increasing specific surface area, the technical problem of its solution is that existing nanofiber does not have great specific area, and manufacturing cost is high simultaneously.
In order to solve the technical problem of above-mentioned existence, the present invention has adopted following scheme:
But a kind of nanofiber of increasing specific surface area, this high surface area nanofibers is nucleocapsid structure, its stratum nucleare is titanium dioxide (TiO
2), shell is tin-antiomony oxide (ATO), shell tin-antiomony oxide (ATO) is SnO
2middle doping Sb element, wherein the quality percentage composition of Sb element is 2O-80%, the nucleocapsid structure that fibre structure is the tin-antiomony oxide cladding titanium dioxide, wherein TiO
2the quality percentage composition be 20-80%, the quality percentage composition of ATO is 20-80%, the nanofiber average diameter of nucleocapsid structure is 100-450nm, it is characterized in that: step 1, butyl titanate and polyvinylpyrrolidone are dissolved in ethanol, stir the stratum nucleare spinning solution that obtains homogeneous; Step 2, stannic chloride pentahydrate, trichloride antimony, polyvinylpyrrolidone are dissolved in DMF, stir the shell layer spinning solution that obtains homogeneous; Step 3, gained spinning solution in step 1 and step 2 is placed in to electrospinning device, the setting spinning head of electrospinning device and dash receiver distance are 15-20cm, the flow velocity of stratum nucleare spinning solution is 0.5-2.0m1/h, and stratum nucleare spinning solution spinnerette diameters is 0.5-1.0mm; The flow velocity of shell layer spinning solution is 0.5-3.0ml/h, and the shell layer spinning solution spinnerette diameters is 1.0-1.5mm; After stable the outflow, applying electrostatic potential is 25kV, and coaxial electrostatic spinning is collected and obtained nonwoven fabric shape fibrofelt; Step 4, gained nonwoven fabric shape fibrofelt in step 3 is calcined under 500 ℃ of-1000 ℃ of conditions to 11-15 hour, obtained the nuclear shell structure nano fiber.
Further, the mass ratio of butyl titanate, polyvinylpyrrolidone and ethanol is 1:1:50-60.
Further, the mass ratio of stannic chloride pentahydrate, trichloride antimony, polyvinylpyrrolidone and DMF is 30-40:20:5:40.
This high surface area nanofibers has following beneficial effect:
(1) the present invention adopts electrostatic spinning technique to prepare nucleocapsid structure (titanium dioxide stratum nucleare/tin-antiomony oxide shell) nanofiber, and the preparation method is simple, and the nano-fiber material of gained has reduced the cost of conductive material, has great specific area.
(2) electrostatic spinning technique of the present invention is that current preparation is continuous, even the most simple and efficient long stapled method, and electrostatic spinning technique can be prepared the nano-scale fiber of diameter at 100-450nm.And electrostatic spinning technique has the advantages such as easy and simple to handle, low-cost, great development prospect and using value are arranged preparing aspect nanofiber.
The accompanying drawing explanation
Fig. 1: the electrospinning device structural representation used in the present invention.
Description of reference numerals:
1-stratum nucleare spinning solution spinning head; The 2-high voltage source; 3-shell layer spinning solution spinning head; The 4-coaxial nozzle; The 5-container; The 6-gathering-device; 7-insulated enclosure lid; Axle transit passage in 8-; 9-sidewall passage.
The specific embodiment
Below in conjunction with Fig. 1 and embodiment, the present invention will be further described:
As shown in Figure 1, electrospinning device comprises stratum nucleare spinning solution spinning head 1, and stratum nucleare spinning solution spinning head 1 is arranged on an end of interior axle transit passage 9, and the other end of interior axle transit passage 9 is arranged in coaxial nozzle 4.Shell layer spinning solution spinning head 3 arranges on sidewall passage 9, sidewall passage 9 communicates with the sidewall of container 5, shell layer spinning solution enters into the coaxial nozzle 4 of container 5 bottoms successively by shell layer spinning solution spinning head 3 and sidewall passage 9, and mixed rear ejection with the stratum nucleare spinning solution, the mixture of stratum nucleare spinning solution and shell layer spinning solution is sprayed onto on gathering-device 6, gathering-device 6 is connected with the negative pole of high voltage source 2, and the positive pole of high voltage source 2 is connected with interior axle transit passage 9, and gathering-device 6 bottoms are ground connection also.
The electrostatic spinning process parameter that the present invention selects: the flow velocity of stratum nucleare spinning solution is 0.5-2.0m1/h, and the flow velocity of shell layer spinning solution is 0.5-3.0m1/h.Flow velocity is excessive, and the droplet size that coaxial nozzle 4 places are not stretched in time is larger, because solvent evaporates is solidified, can stop up coaxial nozzle 4, and flow velocity is too small, and fiber collecting speed is slow, and productive rate is low.
Stratum nucleare spinning solution spinnerette diameters is 0.5-1.0mm.The shell layer spinning solution spinnerette diameters is 1.0-1.5mm.Spinnerette diameters is too little, and polymer solution easily stops up, and spinnerette diameters is too large, easily flows out and produces drippage.The setting spinning head of electrospinning device and dash receiver distance are 15-20cm, receiving range is excessive, before fiber arrives collecting board, solvent fully volatilizees, fiber is owing to excessively stretching and destroying pattern, accept distance too small, after fiber arrives collecting board, due to not fully volatilization of solvent, residual solvent is more, also can destroy the pattern of fiber.
Embodiment 1:
Step 1: measure 50 gram ethanol, 1 gram butyl titanate, 1 gram polyvinylpyrrolidone and mixed in container and stir, obtain homogeneous stratum nucleare spinning solution.
Step 2: take 40g stannic chloride pentahydrate, 20g trichloride antimony, 5g polyvinylpyrrolidone and be dissolved in 40gN, in dinethylformamide, obtain the homogeneous shell layer spinning solution.
Step 3, gained spinning solution in step 1 and step 2 is placed in to electrospinning device, the setting spinning head of electrospinning device and dash receiver distance are 15-20cm, the flow velocity of stratum nucleare spinning solution is 0.5-2.0m1/h, and stratum nucleare spinning solution spinnerette diameters is 0.5-1.0mm; The flow velocity of shell layer spinning solution is 0.5-3.0ml/h, and the shell layer spinning solution spinnerette diameters is 1.0-1.5mm; After stable the outflow, applying electrostatic potential is 25kV, and coaxial electrostatic spinning is collected and obtained nonwoven fabric shape fibrofelt.
Step 4, gained nonwoven fabric shape fibrofelt in step 3 is placed in to the temperature programmed control Muffle furnace, 4 ℃/min of heating rate, be warming up to 700 ℃, and calcining 13h obtains the nanofiber of nucleocapsid structure.
Embodiment 2:
Step 1: measure 60 gram ethanol, 1 gram butyl titanate, 1 gram polyvinylpyrrolidone and mixed in container and stir, obtain homogeneous stratum nucleare spinning solution.
Step 2: take 30g stannic chloride pentahydrate, 20g trichloride antimony, 5g polyvinylpyrrolidone and be dissolved in 40gN, in dinethylformamide, obtain the homogeneous shell layer spinning solution.
Step 3, gained spinning solution in step 1 and step 2 is placed in to electrospinning device, the setting spinning head of electrospinning device and dash receiver distance are 15-20cm, the flow velocity of stratum nucleare spinning solution is 0.5-2.0m1/h, and stratum nucleare spinning solution spinnerette diameters is 0.5-1.0mm; The flow velocity of shell layer spinning solution is 0.5-3.0m1/h, and the shell layer spinning solution spinnerette diameters is 1.0-1.5mm; After stable the outflow, applying electrostatic potential is 25kV, and coaxial electrostatic spinning is collected and obtained nonwoven fabric shape fibrofelt.
Step 4, gained nonwoven fabric shape fibrofelt in step 3 is placed in to the temperature programmed control Muffle furnace, 4 ℃/min of heating rate, be warming up to 800 ℃, and calcining 11h obtains the nanofiber of nucleocapsid structure.
The above has carried out exemplary description to the present invention by reference to the accompanying drawings; obvious realization of the present invention is not subject to the restrictions described above; as long as the various improvement that adopted method design of the present invention and technical scheme to carry out; or without improving, design of the present invention and technical scheme are directly applied to other occasion, all in protection scope of the present invention.
Claims (3)
- But 1. the nanofiber of an increasing specific surface area, this high surface area nanofibers is nucleocapsid structure, its stratum nucleare is titanium dioxide (TiO 2), shell is tin-antiomony oxide (ATO), shell tin-antiomony oxide (AT0) is SnO 2middle doping Sb element, wherein the quality percentage composition of Sb element is 20-80%, the nucleocapsid structure that fibre structure is the tin-antiomony oxide cladding titanium dioxide, wherein Ti0 2the quality percentage composition be 20-80%, the quality percentage composition of ATO is 20-80%, the nanofiber average diameter of nucleocapsid structure is 100-450nm, it is characterized in that: step 1, butyl titanate and polyvinylpyrrolidone are dissolved in ethanol, stir the stratum nucleare spinning solution that obtains homogeneous; Step 2, stannic chloride pentahydrate, trichloride antimony, polyvinylpyrrolidone are dissolved in DMF, stir the shell layer spinning solution that obtains homogeneous; Step 3, gained spinning solution in step 1 and step 2 is placed in to electrospinning device, the setting spinning head of electrospinning device and dash receiver distance are 15-20cm, the flow velocity of stratum nucleare spinning solution is 0.5-2.0m1/h, and stratum nucleare spinning solution spinnerette diameters is 0.5-1.0mm; The flow velocity of shell layer spinning solution is 0.5-3.0m1/h, and the shell layer spinning solution spinnerette diameters is 1.0-1.5mm; After stable the outflow, applying electrostatic potential is 25kV, and coaxial electrostatic spinning is collected and obtained nonwoven fabric shape fibrofelt; Step 4, gained nonwoven fabric shape fibrofelt in step 3 is calcined under 500 ℃ of-1000 ℃ of conditions to 11-15 hour, obtained the nuclear shell structure nano fiber.
- 2. but the nanofiber of increasing specific surface area according to claim 1, it is characterized in that: the mass ratio of butyl titanate, polyvinylpyrrolidone and ethanol is 1:1:50-60.
- 3. but the nanofiber of increasing specific surface area according to claim 1, it is characterized in that: the mass ratio of stannic chloride pentahydrate, trichloride antimony, polyvinylpyrrolidone and DMF is 30-40:20:5:40.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103966691A (en) * | 2014-04-29 | 2014-08-06 | 中原工学院 | Preparation method for nanometer ATO/ cellulose diacetate composite electro-conductive fiber |
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| CN101423634A (en) * | 2008-12-18 | 2009-05-06 | 江南大学 | Method for preparing multifunctional nano composite material |
| CN101763917A (en) * | 2010-03-04 | 2010-06-30 | 长春理工大学 | Method for preparing tin dioxide and titanium dioxide nano cable |
| CN101903182A (en) * | 2007-06-29 | 2010-12-01 | 默克专利股份有限公司 | The microsphere that comprises polymer core, shell and absorbent |
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-
2013
- 2013-08-29 CN CN201310381766.4A patent/CN103436991B/en not_active Expired - Fee Related
Patent Citations (5)
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| CN101903182A (en) * | 2007-06-29 | 2010-12-01 | 默克专利股份有限公司 | The microsphere that comprises polymer core, shell and absorbent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103966691A (en) * | 2014-04-29 | 2014-08-06 | 中原工学院 | Preparation method for nanometer ATO/ cellulose diacetate composite electro-conductive fiber |
| CN103966691B (en) * | 2014-04-29 | 2016-04-13 | 中原工学院 | A kind of preparation method of nano ATO/cellulose diacetate composite conducting fiber |
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| CN103436991B (en) | 2016-06-15 |
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Effective date of registration: 20170921 Address after: 300000 Ningxia Binhai New Area of Tianjin Dongjiang Bonded Port Road No. 666 Kan Hin 5-1-1704 Patentee after: Gao Jianhua Address before: 239001 No. 82 Garden Road West, Anhui, Chuzhou Patentee before: CHUZHOU PINCHUANG BIOTECHNOLOGY Co.,Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160615 |