CN117038983A - Preparation method and application of lithium ion battery binder - Google Patents
Preparation method and application of lithium ion battery binder Download PDFInfo
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- CN117038983A CN117038983A CN202310941937.8A CN202310941937A CN117038983A CN 117038983 A CN117038983 A CN 117038983A CN 202310941937 A CN202310941937 A CN 202310941937A CN 117038983 A CN117038983 A CN 117038983A
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- Prior art keywords
- lithium ion
- ion battery
- negative electrode
- silicon
- binder
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- 239000011230 binding agent Substances 0.000 title claims abstract description 38
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 39
- 239000010703 silicon Substances 0.000 claims abstract description 39
- 239000000017 hydrogel Substances 0.000 claims abstract description 15
- RPHKINMPYFJSCF-UHFFFAOYSA-N benzene-1,3,5-triamine Chemical compound NC1=CC(N)=CC(N)=C1 RPHKINMPYFJSCF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004132 cross linking Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000004584 polyacrylic acid Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 6
- 239000007773 negative electrode material Substances 0.000 claims description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052744 lithium Inorganic materials 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 239000011889 copper foil Substances 0.000 claims description 4
- 239000011267 electrode slurry Substances 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 abstract description 5
- 230000001070 adhesive effect Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000010405 anode material Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000011149 active material Substances 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- -1 lithium hexafluorophosphate Chemical compound 0.000 description 14
- 239000003792 electrolyte Substances 0.000 description 8
- 239000004743 Polypropylene Substances 0.000 description 7
- 229920001155 polypropylene Polymers 0.000 description 7
- 238000011056 performance test Methods 0.000 description 5
- 239000011856 silicon-based particle Substances 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000011863 silicon-based powder Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910015872 LiNi0.8Co0.1Mn0.1O2 Inorganic materials 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920005596 polymer binder Polymers 0.000 description 2
- 239000002491 polymer binding agent Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- 239000006256 anode slurry Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000011263 electroactive material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to a preparation method and application of a lithium ion battery binder. The method comprises the following steps: (1) Dissolving 1,3, 5-triaminobenzene and polyacrylic acid in deionized water, and uniformly stirring at room temperature to obtain a mixed solution; (2) Standing the mixed solution at room temperature to complete the crosslinking reaction to obtain hydrogel; (3) And (3) performing vacuum filtration on the hydrogel obtained in the step (2), and then drying under vacuum conditions to obtain the lithium ion battery binder. The adhesive prepared by the invention can achieve good bonding effect with small dosage when being applied to the silicon-based lithium ion battery anode material, can obviously improve the film forming property of the material, and has the advantages of low price and easy obtainment of raw materials, simple preparation method, environmental friendliness, no pollution and the like. The lithium ion secondary battery prepared by the adhesive has the characteristics of high active material capacity exertion, long cycle service life of the battery and the like.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to a preparation method and application of a lithium ion battery binder.
Background
Silicon is the ideal negative electrode material for lithium ion batteries. On the one hand, the theoretical specific capacity of silicon (4200 mAh g -1 ) Far higher than graphite (372 mAh g) -1 ). On the other hand, the silicon content in the crust is also very rich, and can provide inexhaustible raw materials for the preparation of the lithium ion battery. Therefore, lithium battery silicon negative electrode will be the main energy source equipment in the future. However, silicon undergoes dramatic volume changes during delithiation/intercalation, which in turn leads to the silicon particles themselvesAnd (3) breaking and falling off of the SEI film, so that the SEI film is broken and repeatedly formed, and finally, the electrolyte is seriously consumed. In addition, the film thickness increases in the re-forming process of the SEI film, thereby increasing the internal resistance of the silicon negative electrode and affecting the performance of the lithium ion battery. The rupture of the silicon negative electrode also causes the destruction of the internal structure of the silicon negative electrode, thereby inhibiting the function of the electrode for lithium ion transport. The binder plays an important role in the silicon anode. The adhesive can be connected with the silicon particles and the current collector through the acting forces such as hydrogen bonds, covalent bonds, dipole force and the like, so that the cohesive force of the silicon anode is increased. The improvement of the cohesion of the electrode helps to relieve the expansion and breakage of the silicon particles, thereby reducing the side reactions of the silicon anode during operation. PVDF is applicable as an oily binder for graphite cathodes, but it cannot form a tight bond with silicon particles. The newly researched CMC, SA, GG and other water-based bonding has rich polar groups, and can form strong interaction with Si-OH, thereby relieving the expansion of silicon particles. However, since these binders are long-chain organic substances, agglomeration may occur inside the electrode. Agglomeration of the binder will result in uneven stress distribution to the silicon anode, which is prone to cracking and falling off.
In order to solve the problems, the invention uses the 1,3, 5-triaminobenzene for connecting a plurality of long-chain organic matters, so as to relieve uneven stress and improve the structural stability and the cycle stability of the silicon negative electrode.
In view of the above, the invention provides a preparation method of a lithium ion battery binder, which aims to solve the problem that the stress of a silicon negative electrode is uneven due to agglomeration of a general binder.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a lithium ion battery binder, which adopts 1,3, 5-triaminobenzene to crosslink with a plurality of polyacrylic acid molecules to form macromolecular hydrogel, and the obtained polymer binder has the effect of stress dissipation, reduces uneven stress and improves the structural stability and the cycle stability of a silicon negative electrode.
In order to achieve the above purpose, the present invention provides a method for preparing a lithium ion battery binder, comprising the following steps:
(1) Dissolving 1,3, 5-triaminobenzene and polyacrylic acid (PAA) in deionized water, and uniformly stirring at room temperature to obtain a mixed solution;
(2) Standing the mixed solution at room temperature to complete the crosslinking reaction to obtain hydrogel;
(3) And (3) performing vacuum filtration on the hydrogel obtained in the step (2), and then drying under vacuum conditions to obtain the lithium ion battery binder.
Further, the mass ratio of the 1,3, 5-triaminobenzene to the polyacrylic acid is 0.02-3, and the concentration of the mixed solution is 50g/L-100g/L.
In order to achieve sufficient crosslinking of 1,3, 5-triaminobenzene with polyacrylic acid, the standing time in step (2) is 6-16h, during which the crosslinking is due to-NH in 1,3, 5-triaminobenzene 2 The presence of steric hindrance makes it difficult for self-polymerization to occur, but the polyacrylic acid is linked to-NH 2 The above process realizes the crosslinking reaction of the 1,3, 5-triaminobenzene and the polyacrylic acid to form the macromolecular hydrogel.
Preferably, the temperature of the drying in the step (4) is 80-100 ℃ and the drying time is 1-24h.
The invention further aims to provide an application of the lithium ion battery binder prepared by the method in a lithium battery silicon negative electrode, and the lithium ion battery binder and the silicon-based negative electrode material are mixed to prepare a negative electrode plate of the lithium battery. The silicon powder can be broken in the charging and discharging process, and the silicon powder is combined with the macromolecular binder, so that the silicon powder is integrated with binder molecules even if broken, and the volume expansion is avoided, so that excellent mechanical stability and circulation stability are provided for the silicon negative electrode.
Further, the lithium ion battery binder and the silicon-based negative electrode material are mixed in deionized water to form negative electrode slurry, and then the negative electrode slurry is coated on copper foil, dried and sliced to obtain the silicon negative electrode plate.
The beneficial effects are that:
(1) The invention adopts the 1,3, 5-triaminobenzene to crosslink with a plurality of polyacrylic acid molecules to form macromolecular hydrogel, so as to obtain a polymer binder, and the binder is used for preparing a silicon negative electrode plate, so that the mechanochemical performance between silicon nano particles and the binder is enhanced, the effect of stress dissipation is achieved, the stress non-uniformity is relieved, and the structural stability and the cyclic stability of the silicon negative electrode are improved.
(2) The adhesive prepared by the invention can achieve good bonding effect with little dosage when being applied to the silicon-based lithium ion battery anode material, and can obviously improve the film forming property of the material; when the binder serving as the silicon negative electrode active material is assembled into a lithium ion secondary battery, the lithium ion secondary battery has high cycle stability and good electrochemical performance, and can realize high mechanical strength and long cycle life (500 cycles) of the silicon negative electrode.
(3) The invention has simple operation, low manufacturing cost, simple and convenient required equipment and easy mass production.
Detailed Description
The technical scheme of the present invention is further described below with reference to specific embodiments, but is not limited thereto, and modifications and equivalents of the technical scheme of the present invention should be included in the protection scope of the present invention without departing from the spirit and scope of the technical scheme of the present invention.
The preparation and test processes of the button half-cell of the invention are as follows:
2g of silicon-based anode material (10 nm-60 nm) and 0.05g-1g of prepared binder are mixed in aqueous solution and stirred to form uniform anode slurry. The slurry is uniformly coated on copper foil, then dried at 120 ℃, rolled and punched to prepare the round silicon negative plate. After vacuum drying at 120℃in a glove box (H in the glove box) under a dry argon atmosphere 2 O and O 2 The content of (2) is lower than 0.1 ppm), and the electrolyte is 1M lithium hexafluorophosphate (EC/DMC/EMC=1:1:1 (v)), and the separator is polypropylene.
Example 1
(1) Dissolving 0.5g of 1,3, 5-triaminobenzene and 1g of polyacrylic acid (PAA) in 20mL of deionized water, and uniformly stirring at room temperature to obtain a mixed solution;
(2) Standing the mixed solution for 12 hours at room temperature, wherein the amino groups and the hydroxyl groups form hydrogen bond crosslinking to complete the crosslinking reaction, so as to obtain hydrogel;
(3) And (3) carrying out vacuum filtration on the hydrogel obtained in the step (2), washing with excessive deionized water to remove excessive impurities and byproducts, and drying a filter cake at a temperature of 100 ℃ under vacuum for 12 hours to remove excessive moisture to obtain the lithium ion battery binder.
Example 2
(1) Dissolving 0.5g of 1,3, 5-triaminobenzene and 4g of polyacrylic acid (PAA) in 25mL of deionized water, and uniformly stirring at room temperature to obtain a mixed solution;
(2) Standing the mixed solution at room temperature for 6 hours, wherein the amino groups and the hydroxyl groups form hydrogen bond crosslinking to complete the crosslinking reaction, so as to obtain hydrogel;
(3) And (3) carrying out vacuum filtration on the hydrogel obtained in the step (2), washing with excessive deionized water to remove excessive impurities and byproducts, and drying a filter cake at 80 ℃ for 24 hours under vacuum conditions to remove excessive moisture, thereby obtaining the lithium ion battery binder.
Example 3
(1) 1.5g of 1,3, 5-triaminobenzene and 0.5g of polyacrylic acid (PAA) are dissolved in 30mL of deionized water, and stirred evenly at room temperature to obtain a mixed solution;
(2) Standing the mixed solution at room temperature for 16h, wherein the amino groups and the hydroxyl groups form hydrogen bond crosslinking to complete the crosslinking reaction, so as to obtain hydrogel;
(3) And (3) carrying out vacuum filtration on the hydrogel obtained in the step (2), washing with excessive deionized water to remove excessive impurities and byproducts, and drying a filter cake at 100 ℃ for 6 hours under vacuum conditions to remove excessive moisture, thereby obtaining the lithium ion battery binder.
Example 4
Dissolving 0.05g of the binder prepared in example 1 in 10mL of deionized water, adding 2g of silicon-based negative electrode material (commercially available from Zhejiang iron metal materials Co., ltd.) and stirring to form a negative electrode slurry, uniformly coating the slurry on copper foil, andoven drying at 120deg.C, rolling, punching to obtain round silicon negative plate, vacuum drying at 120deg.C for 12 hr, and placing into a glove box (glove box H) 2 O and O 2 The content of (2) is lower than 0.1 ppm), and the half-cell is assembled by pairing with a metal lithium electrode, 1M lithium hexafluorophosphate is used as electrolyte (EC/DMC/EMC=1:1:1 (v), and a polypropylene separator is used as a separator.
Through tests, the lithium ion half battery prepared by adopting the binder obtained in the embodiment 1 is charged and discharged at the current of 0.5C, the first reversible capacity reaches 3500mAh/g, and the electrode has no material dropping phenomenon. Repeated tests show that the charge and discharge properties of the lithium ion half-cells prepared by using the binders obtained in examples 2-3 are not greatly different from those of example 1.
Example 5
Silicon negative electrode sheet prepared in example 4, liCoO 2 For the positive electrode, a full cell was assembled from a 1M lithium hexafluorophosphate (EC/DMC/emc=1:1:1 (v)) for the electrolyte and a polypropylene separator for the separator, and performance test was performed, and the test results are shown in table 1.
Example 6
Silicon negative electrode sheet prepared in example 4, liMn 2 O 4 For the positive electrode, a full cell was assembled from a 1M lithium hexafluorophosphate (EC/DMC/emc=1:1:1 (v)) for the electrolyte and a polypropylene separator for the separator, and performance test was performed, and the test results are shown in table 1.
Example 7
Silicon negative electrode sheet prepared in example 4, liNi 0.8 Co 0.1 Mn 0.1 O 2 For the positive electrode, a full cell was assembled from a 1M lithium hexafluorophosphate (EC/DMC/emc=1:1:1 (v)) for the electrolyte and a polypropylene separator for the separator, and performance test was performed, and the test results are shown in table 1.
Example 8
The silicon negative electrode sheet prepared in example 4, liFePO 4 For the positive electrode, a full cell was assembled from a 1M lithium hexafluorophosphate (EC/DMC/emc=1:1:1 (v)) for the electrolyte and a polypropylene separator for the separator, and performance test was performed, and the test results are shown in table 1.
Comparative examples 1 to 4
Substitute example with PVDF adhesive4, respectively mixing the silicon negative electrode plate prepared by the adhesive in step 4 with LiCoO 2 、LiMn 2 O 4 、LiNi 0.8 Co 0.1 Mn 0.1 O 2 And LiFePO 4 As a positive electrode, a full cell was assembled, and performance test was performed, and the test results are shown in table 1.
Wherein 1M lithium hexafluorophosphate (EC/DMC/emc=1:1:1 (v)) was used for the electrolyte and polypropylene separator was used for the separator.
TABLE 1 charge and discharge performance parameters and cycle Capacity Retention Rate for various batteries
As can be seen from Table 1, the lithium ion secondary battery assembled by the binder prepared by the method of the invention has the characteristics of high capacity exertion of electroactive materials, long cycle service life of the battery, high voltage of a discharge platform and the like.
The invention is not limited to the above embodiments, and based on the technical solution disclosed in the invention, a person skilled in the art may make some substitutions and modifications to some technical features thereof without creative effort according to the technical content disclosed, and all the substitutions and modifications are within the protection scope of the invention.
Claims (6)
1. The preparation method of the lithium ion battery binder is characterized by comprising the following steps:
(1) Dissolving 1,3, 5-triaminobenzene and polyacrylic acid in deionized water, and uniformly stirring at room temperature to obtain a mixed solution;
(2) Standing the mixed solution at room temperature to complete the crosslinking reaction to obtain hydrogel;
(3) And (3) performing vacuum filtration on the hydrogel obtained in the step (2), and then drying under vacuum conditions to obtain the lithium ion battery binder.
2. The preparation method of the lithium ion battery binder according to claim 1, wherein the mass ratio of the 1,3, 5-triaminobenzene to the polyacrylic acid is 0.02-3, and the concentration of the mixed solution is 50g/L-100g/L.
3. The method for preparing a lithium ion battery binder according to claim 1, wherein the standing time in the step (2) is 6-16 hours.
4. The method for preparing a lithium ion battery binder according to claim 1, wherein the drying temperature in the step (4) is 80-100 ℃ and the drying time is 1-24h.
5. Use of the lithium ion battery binder prepared by the method according to any one of claims 1-4 in a lithium battery silicon negative electrode, wherein the lithium ion battery binder and a silicon-based negative electrode material are mixed for preparing a negative electrode plate of a lithium battery.
6. The use according to claim 5, wherein the lithium ion battery binder and the silicon-based negative electrode material are mixed in deionized water to form a negative electrode slurry, which is then coated on copper foil, and dried and sliced to obtain a silicon negative electrode sheet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310941937.8A CN117038983A (en) | 2023-07-28 | 2023-07-28 | Preparation method and application of lithium ion battery binder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310941937.8A CN117038983A (en) | 2023-07-28 | 2023-07-28 | Preparation method and application of lithium ion battery binder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117038983A true CN117038983A (en) | 2023-11-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310941937.8A Pending CN117038983A (en) | 2023-07-28 | 2023-07-28 | Preparation method and application of lithium ion battery binder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117038983A (en) |
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2023
- 2023-07-28 CN CN202310941937.8A patent/CN117038983A/en active Pending
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Effective date of registration: 20240617 Address after: 213000, Lijiang Road, Xinbei District, Jiangsu, Changzhou, 9 Applicant after: CHAGNZHOU DUBO HIGH-MOLECULAR CO.,LTD. Country or region after: China Address before: 213001 No. 1801 Wu Cheng Road, Changzhou, Jiangsu Applicant before: JIANGSU University OF TECHNOLOGY Country or region before: China |