CN102911419B - Electric hot melt material for plastic welding and preparation method thereof - Google Patents
Electric hot melt material for plastic welding and preparation method thereof Download PDFInfo
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- CN102911419B CN102911419B CN201210398558.0A CN201210398558A CN102911419B CN 102911419 B CN102911419 B CN 102911419B CN 201210398558 A CN201210398558 A CN 201210398558A CN 102911419 B CN102911419 B CN 102911419B
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- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000004023 plastic welding Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000012943 hotmelt Substances 0.000 title abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229920000767 polyaniline Polymers 0.000 claims abstract description 23
- 239000004033 plastic Substances 0.000 claims abstract description 21
- 229920003023 plastic Polymers 0.000 claims abstract description 21
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 5
- 238000007731 hot pressing Methods 0.000 claims abstract description 5
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 5
- 238000000748 compression moulding Methods 0.000 claims abstract description 4
- 238000002844 melting Methods 0.000 claims description 20
- 230000008018 melting Effects 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 19
- 238000005485 electric heating Methods 0.000 claims description 18
- 239000006229 carbon black Substances 0.000 claims description 17
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 6
- 239000004160 Ammonium persulphate Substances 0.000 claims description 5
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000011630 iodine Substances 0.000 claims description 4
- 229910052740 iodine Inorganic materials 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003112 inhibitor Substances 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 3
- 125000003944 tolyl group Chemical group 0.000 claims description 2
- 239000011231 conductive filler Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 229920001940 conductive polymer Polymers 0.000 abstract description 3
- 239000002019 doping agent Substances 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000004804 winding Methods 0.000 abstract description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract 1
- 239000012766 organic filler Substances 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000003466 welding Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- -1 polyethylene Polymers 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 2
- 235000013539 calcium stearate Nutrition 0.000 description 2
- 239000008116 calcium stearate Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000012764 mineral filler Substances 0.000 description 2
- 239000004417 polycarbonate Substances 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920005668 polycarbonate resin Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Lining Or Joining Of Plastics Or The Like (AREA)
Abstract
The invention provides an electric hot melt material for plastic welding and a preparation method thereof. The preparation method comprises the following steps of: (1) performing polymerization reaction at 20-25 DEG C for 6-8 hours by taking hydrochloric acid as a dopant and ammonium persulfate as an oxidant to obtain conductive polyaniline powder; and (2) adding a plastic matrix, the conductive polyaniline powder and conductive carbon black into a mixer to mix for 15-20 minutes according to the proportion of 65-90:5-15:3-10, then performing hot pressing in a plate vulcanizing machine for 20-30 minutes and performing compression molding to obtain a plastic welding connecting piece. According to the invention, high molecular conductive polymer is introduced into conductive filler, so that the content of the organic filler can be greatly reduced, the mechanical property of the plastic connecting piece is improved, and meanwhile, the positive temperature coefficient effect can be effectively controlled through winding action of a macromolecular chain.
Description
Technical field
What the present invention relates to is a kind of Plastic Welding material, particularly relates to a kind of electric heating melting material connecting for plastic component and preparation method thereof.
Background technology
Thermoplastics and matrix material thereof, because having the plurality of advantages such as designability is strong, specific tenacity is high, solidity to corrosion is good, the manufacturing cycle is short, have been widely used in the industries such as aerospace, automobile boats and ships, electronic apparatus, petrochemical complex.But due to the restriction of the factors such as Shooting Technique, complex-shaped goods can not single injection-molded, must carry out secondary and connect processing.At present, the method that plastics connect is a lot, and wherein electric fusion welding is because constructing operation is simple, welding speed is fast, the good developed and popularization in many countries of welding effect.Traditional electric fusion welding method is to adopt the wire resistance that is embedded in plastic fastening by plastic component surface heating, makes plastic molting and merges each other, thereby realizing welding.Conventionally, above-mentioned web member is to adopt the method for injection molding on heater strip to manufacture, before molded or in process, easily there is the danger that heater strip expands and moves, the generation of these displacements, can cause that heat distribution is inhomogeneous, may in web member, produce bubble, also exist because overlapping each other the danger that causes short circuit, this all can reduce welding quality and even cause welding unsuccessfully.
Publication number is: in the patent document of CN1047827A, CN1083767A and CN201827577U, disclosing to relate to adopts the alternative above-mentioned wire of conductive plastics to make resistance heating material, conductive plastics is comprised of plastic substrate and conductive filler material, and conductive filler material is got carbon black or metal and powdered alloy thereof.For meeting the power input of welding requirements, often the content of conductive filler material will reach more than 30%, but too high mineral filler meeting brings obvious disadvantageous effect to the mechanical property of conductive plastics, can limit shape and the operation of above-mentioned web member.
Summary of the invention
The object of the present invention is to provide a kind of electric heating melting material for Plastic Welding that can meet Plastic Welding requirement, there is excellent mechanical performances.The present invention also aims to provide a kind of preparation method of the electric heating melting material for Plastic Welding.
The object of the present invention is achieved like this:
Electric heating melting material for Plastic Welding of the present invention, comprises plastic substrate, electrically conductive polyaniline and graphitized carbon black, and the mass percent of each component is 65 ~ 90 ﹕ 5 ~ 15 ﹕ 3 ~ 10.
Electric heating melting material for Plastic Welding of the present invention also comprises dispersion agent and oxidation inhibitor, and mass percent is 0 ~ 1 ﹕ 0 ~ 0.2.Described dispersion agent is Zinic stearas, calcium stearate or barium stearate.
The preparation method of the electric heating melting material for Plastic Welding of the present invention is: (1) makes doping agent with hydrochloric acid, and ammonium persulphate is made oxygenant, in 20 ~ 25 ℃ of polyreactions 6 ~ 8 hours, obtains electrically conductive polyaniline powder; (2) according to mass percent, be: the ratio of 65 ~ 90 ﹕ 5 ~ 15 ﹕ 3 ~ 10, plastic substrate and electrically conductive polyaniline powder and graphitized carbon black are successively added to mixing 15-20 minute in mixing roll, hot pressing 20-30min in vulcanizing press again, compression molding obtains having the electric heating melting material of certain size, i.e. Plastic Welding web member.Described plastic substrate is polyethylene, polypropylene, polycarbonate or ABS resin.
The preparation method of the electric heating melting material for Plastic Welding of the present invention can also comprise
1, according to mass percent be 0 ~ 1 ﹕ 0 ~ 0.2 ratio to add in mixing roll carry out again after dispersion agent and antioxygen mixing.
2, described electrically conductive polyaniline powder is to adopt with the following method to obtain: at 20 ~ 25 ℃, measure underpressure distillation aniline 5 ~ 10ml and add in container, add 8 ~ 10ml concentrated hydrochloric acid, with distilled water proportioning to 160 ~ 200ml, with ultrasonoscope ultrasonic half an hour; Slowly drip ammonium persulfate solution, room temperature reaction 6 ~ 8 hours; Filter, washing, vacuum-drying, obtains doped hydrochloride polyaniline; Again doped hydrochloride polyaniline is dissolved in 80 ~ 100ml organic solvent, centrifugal, get supernatant liquid as the seed of next step polymerization; Get 4 ~ 5ml aniline and join in 50ml hydrochloric acid soln, add 10 ~ 15ml seed solution, drip the hydrochloric acid soln of ammonium persulphate, under room temperature, react 6 ~ 8 hours, suction filtration, washing, under room temperature, vacuum-drying obtains electrically conductive polyaniline powder for 24 hours.
3, with sulfuric acid, perchloric acid or p-methyl benzenesulfonic acid Instead of Hydrochloric; Described organic solvent is toluene or methyl-sulphoxide.
4, described graphitized carbon black meets following condition: depending on specific volume, be 5.0-7.0cm
3/ g; PH value 8-9; Iodine absorption value: 650g/kg; Resistivity 0.4-0.6 Ω cm.
The present invention imports conductive polymer polymkeric substance in conductive filler material, can greatly reduce the content of mineral filler, improves the mechanical property of plastic fastening, can effectively control positive temperature coefficient effect by the winding effect of macromolecular chain simultaneously.
The present invention compares and has the following advantages with currently available technology: take conductive polymers polyaniline and graphitized carbon black as conductive filler material, bring into play the synergy of the two, can greatly promote the electroconductibility of conducing composite material, obtain good electricity and cause heating property; Solve the problem that conventional filler loading level is large, poor with plastic substrate consistency, the electric heating melting stability of material of preparation is good; Adopt general plastic working method, preparation technology is simple, with low cost, is easy to realize suitability for industrialized production.
Embodiment
For example the present invention is described in more detail below.
1. electrically conductive polyaniline powder is synthetic
At 20 ~ 25 ℃, measure underpressure distillation aniline 5 ~ 10ml and add in there-necked flask, add 8 ~ 10ml concentrated hydrochloric acid, with distilled water proportioning to 160 ~ 200ml, with ultrasonoscope ultrasonic half an hour.Slowly drip ammonium persulfate solution, room temperature reaction 6 ~ 8 hours.Filter, washing, vacuum-drying, obtains doped hydrochloride polyaniline.Be dissolved in again in 80 ~ 100ml organic solvent (toluene, methyl-sulphoxide etc.), centrifugal, get supernatant liquid as the seed of next step polymerization.Get 4 ~ 5ml aniline and join in 50ml hydrochloric acid soln, add 10 ~ 15ml seed solution, drip the hydrochloric acid soln of ammonium persulphate, under room temperature, react 6 ~ 8 hours.Suction filtration, washing, under room temperature, vacuum-drying is 24 hours.Protonic acid is available sulfuric acid, perchloric acid, p-methyl benzenesulfonic acid etc. also.
2. the selection of carbon black
In all conductive filler materials, carbon black with its wide material sources, cheap, conductivity is good and well received.The leading indicator that affects carbon black filled conducing composite material performance has: structural, particle diameter, specific surface area, surface chemical property etc.In this research, selected structure is flourishing, granularity is little, surface polarity group is less graphitized carbon black as conductive filler material, graphitized carbon black used depending on specific volume, be 5.0-7.0cm
3/ g; PH value 8-9; Iodine absorption value: 650g/kg; Resistivity 0.4-0.6 Ω cm.
3. the preparation of electric heating melting material
(1) preheating mixing roll, sets the Heating temperature of mixing roll higher than the melting temperature 10-20 ℃ of plastic substrate; Treat that mixing roll reaches design temperature, first add resin (polyethylene, polypropylene, polycarbonate, ABS resin etc.) 25 ~ 30g and dispersion agent (Zinic stearas, calcium stearate, barium stearate etc.) 1.7 ~ 2g, mixing for some time, when resin presents viscous state, can slowly add polyaniline powder 2.5 ~ 4g, make it fully mixing evenly; And then add resin 10 ~ 15g, then add carbon black 3 ~ 4g, until each component is all mixing complete, mixing time is approximately 15 ~ 20min.
(2) after mixing through 3 ~ 5 times, get mixing thing and put into mould, hot pressing 20 ~ 30min in vulcanizing press, molding temperature is higher than melting point resin temperature 10-20 ℃, and pressure 15MPa obtains the test sample of 60 * 15 * 3mm.
Electricity causes heating property and detects
For meeting Plastic Welding requirement, loading under safety voltage, adopt self-assembly circuit, the electricity of having tested gained print (ABS resin 85%, polyaniline 10%, carbon black 5%) causes heating property, in Table 1.
Electric heating melting material heating situation under table 1 28V voltage
| Test duration/S | Temperature/℃ | Resistance/Ω | Electric current/mA |
| 0 | 25 | 875.2 | 32 |
| 15 | 29 | 824.6 | 35 |
| 30 | 37 | 756.3 | 37 |
| 45 | 44 | 712.6 | 39 |
| 60 | 53 | 687.4 | 41 |
| 75 | 61 | 602.4 | 46 |
| 90 | 69 | 563.2 | 50 |
| 105 | 80 | 487.3 | 57 |
| 120 | 95 | 430.2 | 65 |
| 135 | 114 | 376.5 | 74 |
| 150 | 146 | 307.6 | 91 |
Claims (5)
1. the electric heating melting material for Plastic Welding, it is characterized in that: it is that the mass percent of the plastic substrate, electrically conductive polyaniline and the graphitized carbon black that make is as follows the electric heating melting material for Plastic Welding of 65～90 ﹕ 5～15 ﹕ 3～10, and each component sum is absolutely:
At 20～25 ℃, measure underpressure distillation aniline 5～10ml and add in container, add 8～10ml concentrated hydrochloric acid, with distilled water proportioning to 160～200ml, with ultrasonoscope ultrasonic half an hour; Slowly drip ammonium persulfate solution, room temperature reaction 6～8 hours; Filter, washing, vacuum-drying, obtains doped hydrochloride polyaniline; Again doped hydrochloride polyaniline is dissolved in 80～100ml organic solvent, centrifugal, get supernatant liquid as the seed of next step polymerization; Get 4～5ml aniline and join in 50ml hydrochloric acid soln, add 10～15ml seed solution, drip the hydrochloric acid soln of ammonium persulphate, under room temperature, react 6～8 hours, suction filtration, washing, under room temperature, vacuum-drying obtains electrically conductive polyaniline powder for 24 hours;
According to mass percent, be: the ratio of 65～90 ﹕ 5～15 ﹕ 3～10, plastic substrate and electrically conductive polyaniline powder and graphitized carbon black are successively added to mixing 15-20 minute in mixing roll, hot pressing 20-30min in vulcanizing press again, compression molding, described graphitized carbon black meets following condition: depending on specific volume, be 5.0-7.0cm
3/ g; PH value 8-9; Iodine absorption value: 650g/kg; Resistivity 0.4-0.6 Ω cm.
2. the electric heating melting material for Plastic Welding according to claim 1, is characterized in that: also comprise dispersion agent and oxidation inhibitor, mass percent is 0～1 ﹕ 0～0.2.
3. a preparation method for the electric heating melting material for Plastic Welding as claimed in claim 1, is characterized in that:
(1) at 20～25 ℃, measure underpressure distillation aniline 5～10ml and add in container, add 8～10ml concentrated hydrochloric acid, with distilled water proportioning to 160～200ml, with ultrasonoscope ultrasonic half an hour; Slowly drip ammonium persulfate solution, room temperature reaction 6～8 hours; Filter, washing, vacuum-drying, obtains doped hydrochloride polyaniline; Again doped hydrochloride polyaniline is dissolved in 80～100ml organic solvent, centrifugal, get supernatant liquid as the seed of next step polymerization; Get 4～5ml aniline and join in 50ml hydrochloric acid soln, add 10～15ml seed solution, drip the hydrochloric acid soln of ammonium persulphate, under room temperature, react 6～8 hours, suction filtration, washing, under room temperature, vacuum-drying obtains electrically conductive polyaniline powder for 24 hours;
(2) according to mass percent, be: the ratio of 65～90 ﹕ 5～15 ﹕ 3～10, plastic substrate and electrically conductive polyaniline powder and graphitized carbon black are successively added to mixing 15-20 minute in mixing roll, hot pressing 20-30min in vulcanizing press again, compression molding obtains Plastic Welding web member, and described graphitized carbon black meets following condition: depending on specific volume, be 5.0-7.0cm
3/ g; PH value 8-9; Iodine absorption value: 650g/kg; Resistivity 0.4-0.6 Ω cm.
4. the preparation method of the electric heating melting material for Plastic Welding according to claim 3, is characterized in that: according to mass percent, be 0～1 ﹕ 0～0.2 ratio to add in mixing roll carry out again after dispersion agent and oxidation inhibitor mixing.
5. according to the preparation method of the electric heating melting material for Plastic Welding described in claim 3 or 4, it is characterized in that: with sulfuric acid, perchloric acid or p-methyl benzenesulfonic acid Instead of Hydrochloric; Described organic solvent is toluene or methyl-sulphoxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210398558.0A CN102911419B (en) | 2012-10-19 | 2012-10-19 | Electric hot melt material for plastic welding and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210398558.0A CN102911419B (en) | 2012-10-19 | 2012-10-19 | Electric hot melt material for plastic welding and preparation method thereof |
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| Publication Number | Publication Date |
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| CN102911419A CN102911419A (en) | 2013-02-06 |
| CN102911419B true CN102911419B (en) | 2014-11-05 |
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| CN103146118A (en) * | 2013-02-22 | 2013-06-12 | 哈尔滨工程大学 | Conductive polymer containing conductive polyaniline and plastic welding method by using conductive polymer as heat production source |
| CN104530562A (en) * | 2014-12-24 | 2015-04-22 | 陈程 | High-strength PP (polypropylene) conducting composite material and preparation method thereof |
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| CN102212244B (en) * | 2011-05-05 | 2013-02-06 | 哈尔滨工程大学 | Electroconductive plastic with high electrical conductivity and preparation method thereof |
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Inventor after: Li Ruiqi Inventor after: Chen Zheng Inventor after: Guo Qing Inventor after: Yan Han Inventor after: Li Jiani Inventor before: Li Ruiqi Inventor before: Chen Zheng Inventor before: Guo Qing Inventor before: Li Jiani |
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Effective date of registration: 20201126 Address after: Area A129, 4th floor, building 4, Baitai Industrial Park, Yazhou Bay science and Technology City, Yazhou District, Sanya City, Hainan Province, 572024 Patentee after: Nanhai innovation and development base of Sanya Harbin Engineering University Address before: 150001 Heilongjiang, Nangang District, Nantong street,, Harbin Engineering University, Department of Intellectual Property Office Patentee before: HARBIN ENGINEERING University |
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