CN102980845B - Method for accelerating color printing iron corrosion by using electrochemical cathodic polarization - Google Patents
Method for accelerating color printing iron corrosion by using electrochemical cathodic polarization Download PDFInfo
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- CN102980845B CN102980845B CN201210529625.8A CN201210529625A CN102980845B CN 102980845 B CN102980845 B CN 102980845B CN 201210529625 A CN201210529625 A CN 201210529625A CN 102980845 B CN102980845 B CN 102980845B
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Abstract
The invention provides a method for accelerating color printing iron corrosion by using electrochemical cathodic polarization. The method comprises the following steps of: (1) manufacturing the color printing iron into a working electrode, installing the working electrode into an electrolytic tank, wherein a reference electrode and an auxiliary electrode are installed in the electrolytic tank in advance, and assembling into an electrolytic tank system; (2) maintaining the electrolytic tank system in an anaerobic environment; (3) connecting the electrolytic tank, an electrochemical working station, an adjustable voltage-stabilized power supply and a double-pole-double-throw switch; and (4) adjusting the output voltage of the adjustable voltage-stabilized power supply so as to carry out cathodic polarization on the working electrode, measuring the electrochemical impedance spectrum of the working electrode by using the electrochemical working station, obtaining the coating resistance of the working electrode, and confirming that the coating corrosion final point is reached when the coating resistance is less than or equal to 106omegacm<2>. By utilizing the method, relatively high resolution is achieved, the degree of degradation and failure of the coating is quantitatively analyzed according to the change of the impedance response, and good foundation is established for further improving and optimizing a color printing iron machining process.
Description
Technical field
The present invention relates to a kind of method that electrochemistry color printing iron rot accelerates, particularly relate to a kind of electrochemical cathode that utilizes and to polarize the method that color printing iron rot is accelerated.
Background technology
The beverage of tinplate built-up tin or the shelf life of food, generally at 1-3, because the liquid in metallic beverage can has corrosivity usually, make metallic beverage can be easy to cause with the liquid generation electrochemical reaction in its tank the corrosion of metallic beverage can.When the corrosion condition of metal beverage tank body coating (such as, the beverage can that color printing iron is made) exceedes to a certain degree, product can be made to go bad at shelf-life internal cause coating failure.Therefore, to selecting the coating putting on color printing iron, monitoring and promote its corrosion strength, is one of key factor ensureing product quality.But get rid of the impact of cause specific or human factor, the speed of color printing iron generation spontaneous corrosion is comparatively slow, and the time is longer, only by tracking monitor, cost and efficiency and the sense cycle obtaining conclusion are all difficult to meet the demand of research and development of products and popularization.In order to improve the efficiency detected color printing iron material corrosion resistance, need to adopt accelerated test method to detect the corrosion resistance life-span of color printing iron.
Conventional method clear stipulaties in " QB/T 2763-2006 apply zinc-plated (or chromium) sheet metal " of color printing iron corrosion strength assessment: the size and number of tested print being carried out in simulated test liquid observation print Staining after DC anode polarization, thus obtain the semi-quantitative assessment of corrosion resistance grade.The essence of this corrosion strength method of testing is the method that noble polarization curve accelerates, and the erosion profile of the print that detects by an unaided eye, this judgment criteria not only resolution pole is low, and because of the resolution of observer and deposit index difference, the conclusion drawn obviously exists the risk of erroneous judgement.
Therefore, how to provide a kind of accelerated test method to detect the corrosion resistance life-span of color printing iron, and the method has higher resolution ratio, and then evaluate the barrier propterty of coating and corrosion life and become and have problem to be solved.
Summary of the invention
The object of the invention is to solve above-mentioned technical problem, provide a kind of electrochemical cathode that utilizes to polarize the method that color printing iron rot is accelerated, the method has higher resolution ratio, by measuring the impedance response of whole corrosion process, and the degree of quantitative analysis coating degradations and inefficacy is determined according to the change of impedance response, lay good basis for improving and optimize color printing ironworking technique further.
The invention provides a kind of electrochemical cathode that utilizes to polarize the method that color printing iron rot is accelerated, the method comprises the following steps:
1) color printing iron is made working electrode, be installed in electrolytic cell, in this electrolytic cell, reference electrode and auxiliary electrode are installed in advance, and be assembled into electrolytic cell system;
2) make described in be provided with working electrode, reference electrode and auxiliary electrode electrolytic cell system keep oxygen-free environment;
3) connect electrolytic cell, electrochemical workstation, adjustable stabilized voltage supply and double-point double-throw switch, and be connected with working electrode by the negative pole of adjustable stabilized voltage supply, positive pole is connected with auxiliary electrode;
4) regulate the output voltage of adjustable stabilized voltage supply to carry out cathodic polarization to working electrode, and use electrochemical workstation to measure its electrochemical impedance spectroscopy, and obtain the coating resistance of working electrode, when described coating resistance is less than or equal to 10
6Ω .cm
2, determine to reach coating corrosion terminal.
The working electrode material selection used in the present invention is as the color printing iron of metal packing material.Usually used as working electrode, use its surface of alcohol washes before the use, the oil stain on removing surface and impurity.
Reference electrode described in the present invention adopts solid calomel reference electrode or solid Ag/AgCl reference electrode; Described auxiliary electrode adopts platinum plate electrode, platinized titanium net electrode, stainless steel substrates or graphite flake electrode.Needed to correct it before use reference electrode, the reference electrode used in the present invention utilizes conventional bearing calibration to correct; Needed to carry out polishing to it before use auxiliary electrode, usually utilize sand papering to remove the oxide on surface.Those skilled in the art can according to the auxiliary electrode of the different choice suitable type of the difference of metal packing material to be detected and electrolyte and reference electrode, as long as the corrosion resistance that can meet metal packing material to be detected detects needs.
In the inventive solutions, the output voltage of adjustable stabilized voltage supply is regulated to carry out cathodic polarization in-4V to-10V scope.Usually, metallic beverage can corrosion process can experience several stage with Corrosion Electrochemical Characteristics such as coating infiltration, metallic substrates burn into coating bubbling cracking, corrosion propagation successively, and activation polarization can slow down or accelerated corrosion process.Preliminary experiment shows, the cathodic polarization of about-1.0V can produce cathodic protection effect, slows down Process of Metallic Corrosion; And-3V or the potential region more negative than this value, lost efficacy because the cathodic processes such as cation permeability, liberation of hydrogen and hydrogen reduction can accelerate coating degradations, thus accelerated the corrosion process of metal can.
In the inventive solutions, measure in the process of its electrochemical impedance spectroscopy at electrochemical workstation, arranging sine wave disturbance signal initial frequency is 99KHz, and termination frequency is 9mHz, and disturbance current potential is 5-30mV.
According to the specific embodiment of the present invention, repeat electrochemical cathode polarization by one or many and electrochemical impedance measurement realizes coating resistance and is less than or equal to 10
6Ω .cm
2.Corrosion process progress extent depends on corrosion area and corrosion strength, is compared to corroded area and hot spot quantitative approach, adopts coating resistance to drop to 10
6Ω .cm
2more reasonable and accurate as corrosion life endpoint criteria.
The simulated solution of the food liquid that the electrolyte in the present invention program will be packed for described metal packing material to be detected or non-liquid food, described simulated solution is the solution be made into according to the chemical composition of described non-liquid food, such as, do not contain or contain various fruit juice, tea beverage, milk, the tomato dip of minute quantity solid insoluble (not affecting the formation of electron stream in electrolyte).
Whole electrolytic cell system is kept to be in oxygen-free environment in the present invention program, the normally used inert gas of food and drink packaging process can be passed into, also can be the nitrogen etc. of high-purity (more than 99.99v/v%), as long as can ensure that the whole electrolytic cell system of testing process is in anaerobic state.
Compared with prior art, technical scheme of the present invention has following beneficial effect:
1, the present invention utilizes electrochemical cathode to polarize the method that color printing iron rot is accelerated, and effectively can accelerate the speed of coating corrosion, the Corrosion results of accurate evaluation color printing iron.
2, the present invention utilizes electrochemical cathode to polarize the method that color printing iron rot is accelerated, its test have highly sensitive, resolution ratio is high, and can by measuring the information such as the integrality of coating resistance electrolytic coating and inefficacy.
3, can according to the evaluation result of color printing iron accelerated corrosion, the effective processing technology improved and optimize color printing iron.
Accompanying drawing explanation
Fig. 1 is the structural representation of electrolytic cell of the present invention.
Fig. 2 is electrochemical cathode polarization color printing iron rot acceleration test apparatus figure.
Fig. 3 (a)-Fig. 3 (b) is the Bode figure and erosion profile figure of color printing iron under-4.414V cathodic polarization potential.
Fig. 4 is the Bode figure of color printing iron under-6.414V cathodic polarization potential.
Fig. 5 (a)-Fig. 5 (b) is the Bode figure and erosion profile figure of color printing iron under-7.414v cathodic polarization potential.
Fig. 6 (a)-Fig. 6 (b) is the Bode figure and erosion profile figure of color printing iron under-8.414v cathodic polarization potential.
Fig. 7 is the change curve of color printing iron corrosion resisting property with cathodic polarization potential.
The explanation of symbol:
1: to contact conductor, 2: reference electrode goes between, 3: inert gas inleting pipe, 4: air discharge duct, 5: to electrode, 6: reference electrode, 7: sealing ring, 8: bottom (i.e. working electrode: precoated metal packaging material to be detected), 9: base, 10: bolt, 11: working electrode goes between, 12: upper cover.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with specific embodiment, technical scheme of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
1, the preparation of instrument
About the electrode used in the present invention and electrolytic cell, the earlier application CN201210172244.9 of applicant in this case, in denomination of invention " a kind of electrolytic cell for detecting packaging material corrosion resistance ", all have a detailed description, this case is incorporated to the part as the application.
According to Fig. 1, electrolytic cell and electrode are installed.Color printing iron working electrode is put in bottom pipe dress electrolytic cell, working face is set up, rubber sealing, install upper cover, screw 4 bolts, loading reference electrode and auxiliary electrode are in place, air induction hose and exhaust hose are installed, open nitrogen valve, adjust flux is 2 bubbles per second, keeps nitrogen deoxygenation.Reference electrode lower end is fit in Luggin capillary, regulates side on the working electrode (s, Luggin capillary end, contacts working electrode and can not have the bubble of isolation circuitry in Luggin capillary.
As shown in Figure 2, electrolytic cell, electrochemical workstation, adjustable stabilized voltage supply and double-point double-throw switch is connected.The negative pole of adjustable stabilized voltage supply is connected to working electrode, and positive pole is connected to auxiliary electrode; Working electrode connects the W lead-out terminal of electrochemical workstation, and reference electrode connects the R lead-out terminal of electrochemical workstation, and auxiliary electrode connects the C lead-out terminal of electrochemical workstation.
In this experiment, working electrode is that red drink heavily batch can is cut into the foursquare color printing iron of 6cm × 6cm, and reference electrode is solid calomel reference electrode, and auxiliary electrode is stainless steel substrates, and electrolyte is red drink heavily material.
Open adjustable stabilized voltage supply, NOVA1.6 function software and electrochemical workstation (Switzerland ten thousand is logical to produce), carry out preheating 10 minutes.
2, operating procedure
1) electrochemical cathode polarization
First regulate the output voltage of adjustable stabilized voltage supply to be-4.414V during electrochemical cathode polarization, then switch is placed in left end, cathodic polarization is carried out to working electrode.
2) measurement of electrochemical impedance spectroscopy
After the polarization of parallel testing electrochemical cathode 0h, 1.5h, 3.5h, 5.5h, 7.5h, 9.5h, 26.5h, the double-point double-throw switch right side is put, after stablizing certain hour, electrochemical workstation (Switzerland ten thousand is logical to produce) is used to measure the electrochemical impedance spectroscopy of above-mentioned cathodic polarization time respectively.
Electrochemical impedance spectroscopy measuring method used in the present invention is consistent with the assay method of prior art, and wherein, setting sine wave disturbance signal initial frequency is 99kHz, and sine wave disturbance signal terminating frequency is 9mHz, and disturbance current potential is 10mV.
3, result judges
Start the chemical impedance spectrum Parameter analysis of electrochemical software of ten thousand energisings, according to the program computation coating resistance of electrochemical impedance spectroscopy Parameter analysis of electrochemical software.
If the coating resistance once measured does not drop to 10
6Ω .cm
2, cathodic polarization accelerated corrosion and the electrochemical impedance that can repeat more than secondary measure operation, until coating resistance drops to 10
6Ω .cm
2, can think coating failure.The output voltage that Fig. 3 (a)-Fig. 3 (b) is adjustable stabilized voltage supply is the Bode figure and erosion profile figure of working electrode under-4.414V.As can be seen from Fig. 3 (a)-Fig. 3 (b), after cathodic polarization in 26.5 hours, the coating of red drink heavily batch can substantially lost efficacy, and Staining is high-visible.
Embodiment 2
Except being that-6.414V replaces-4.414V, replaces except 0h, 1.5h, 3.5h, 5.5h, 7.5h, 9.5h, 26.5h with electrochemical cathode polarization time 0h, 1.5h, 4.5h, 6.5h, 9h, 10.5h, 22.5h with the output voltage of adjustable stabilized voltage supply, all the other are according to method similarly to Example 1.
The Bode figure of Fig. 4 to be the output voltage of adjustable stabilized voltage supply be working electrode under-6.414V.As seen from Figure 4, after cathodic polarization in 22.5 hours, the coating of red drink heavily batch can substantially lost efficacy.
Embodiment 3
Except being that-7.414V replaces-4.414V, replaces except 0h, 1.5h, 3.5h, 5.5h, 7.5h, 9.5h, 26.5h with electrochemical cathode polarization 0h, 1.5h, 3.5h, 5h, 9.5h, 22.5h with the output voltage of adjustable stabilized voltage supply, all the other are according to method similarly to Example 1.
The output voltage that Fig. 5 (a)-Fig. 5 (b) is adjustable stabilized voltage supply is the Bode figure and erosion profile figure of working electrode under-7.414V.As can be seen from Fig. 5 (a)-Fig. 5 (b), after cathodic polarization in 5 hours, the coating of red drink heavily batch can substantially lost efficacy, and Staining is high-visible.
Embodiment 4
Except being that-8.414V replaces-4.414V, replaces except 0h, 1.5h, 3.5h, 5.5h, 7.5h, 9.5h, 26.5h with electrochemical cathode polarization 0h, 1h, 2h, 3.5h, 5h, 6.5h, 8h, 10h with the output voltage of adjustable stabilized voltage supply, all the other are according to method similarly to Example 1.
The output voltage that Fig. 6 (a)-Fig. 6 (b) is adjustable stabilized voltage supply is the Bode figure and erosion profile figure of working electrode under-8.414V.As can be seen from Fig. 6 (a)-Fig. 6 (b), after cathodic polarization in 10 hours, the coating of red drink heavily batch can substantially lost efficacy, and Staining is high-visible.
Fig. 7 is the change curve of color printing iron corrosion resisting property with cathodic polarization potential, can be seen by this figure, along with the increase of cathode potential, can accelerate the speed of color printing iron rot.
Last it is noted that above embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (4)
1. utilize electrochemical cathode to polarize the method that color printing iron rot is accelerated, it is characterized in that, the method comprises the following steps:
1) color printing iron is made working electrode, be installed in electrolytic cell, in this electrolytic cell, reference electrode and auxiliary electrode are installed in advance, and be assembled into electrolytic cell system;
2) make described in be provided with working electrode, reference electrode and auxiliary electrode electrolytic cell system keep oxygen-free environment;
3) connect electrolytic cell, electrochemical workstation, adjustable stabilized voltage supply and double-point double-throw switch, and be connected with working electrode by the negative pole of adjustable stabilized voltage supply, positive pole is connected with auxiliary electrode;
4) regulate the output voltage of adjustable stabilized voltage supply to carry out cathodic polarization to working electrode, and use electrochemical workstation to measure its electrochemical impedance spectroscopy, and obtain the coating resistance of working electrode, when described coating resistance is less than or equal to 10
6Ω .cm
2, determine to reach coating corrosion terminal;
Electrolyte is the simulated solution of food liquid or non-liquid food;
Wherein, regulate the output voltage of adjustable stabilized voltage supply between-4V to-10V.
2. the electrochemical cathode that utilizes according to claim 1 polarizes the method that color printing iron rot is accelerated, and it is characterized in that, described reference electrode adopts solid calomel reference electrode or solid Ag/AgCl reference electrode; Described auxiliary electrode adopts platinum plate electrode, platinized titanium net electrode, stainless steel substrates or graphite flake electrode.
3. the electrochemical cathode that utilizes according to claim 1 polarizes the method that color printing iron rot is accelerated, it is characterized in that, measure in the process of its electrochemical impedance spectroscopy at electrochemical workstation, arranging sine wave disturbance signal initial frequency is 99KHz, termination frequency is 9mHz, and disturbance current potential is 5-30mV.
4. the electrochemical cathode that utilizes according to claim 1 polarizes the method that color printing iron rot is accelerated, and it is characterized in that, repeats electrochemical cathode polarization and electrochemical impedance measurement realize coating resistance and be less than or equal to 10 by one or many
6Ω .cm
2.
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| CN201210529625.8A CN102980845B (en) | 2012-12-10 | 2012-12-10 | Method for accelerating color printing iron corrosion by using electrochemical cathodic polarization |
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| CN102980845B true CN102980845B (en) | 2015-04-29 |
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| CN104502263B (en) * | 2014-12-16 | 2017-06-16 | 哈尔滨工业大学 | Steel and concrete structure cathodic corrosion control anode material acceleration test apparatus and life-span prediction method |
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| GB1150416A (en) * | 1966-07-29 | 1969-04-30 | Nat Res Dev | A Method for the Determination of Corrosion Rates by A.C. Polarisation Resistance Measurement |
| US6365034B1 (en) * | 1997-05-07 | 2002-04-02 | Polymer Alloys Llc | High throughput electrochemical test for measuring corrosion resistance |
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| CN102706795A (en) * | 2012-05-29 | 2012-10-03 | 奥瑞金包装股份有限公司 | Electrolytic tank for detecting corrosion resistance of packing material |
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2012
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1150416A (en) * | 1966-07-29 | 1969-04-30 | Nat Res Dev | A Method for the Determination of Corrosion Rates by A.C. Polarisation Resistance Measurement |
| US6365034B1 (en) * | 1997-05-07 | 2002-04-02 | Polymer Alloys Llc | High throughput electrochemical test for measuring corrosion resistance |
| CN1474174A (en) * | 2002-08-19 | 2004-02-11 | 乐金电子(天津)电器有限公司 | Detecting sysytem for metal corrosion resistance |
| CN102706795A (en) * | 2012-05-29 | 2012-10-03 | 奥瑞金包装股份有限公司 | Electrolytic tank for detecting corrosion resistance of packing material |
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Address after: 101407 Beijing Huairou District wild goose Industrial Development Zone Patentee after: Origen Polytron Technologies Inc Address before: 101407 No. 7 Nan Yi Street, Yan Xi economic development zone, Huairou District, Beijing Patentee before: ORG Packaging Co., Ltd. |
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