CN113912742A - Synthesis method of lithium carboxymethyl cellulose with ultrahigh substitution degree and ultrahigh viscosity - Google Patents
Synthesis method of lithium carboxymethyl cellulose with ultrahigh substitution degree and ultrahigh viscosity Download PDFInfo
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- CN113912742A CN113912742A CN202111041757.1A CN202111041757A CN113912742A CN 113912742 A CN113912742 A CN 113912742A CN 202111041757 A CN202111041757 A CN 202111041757A CN 113912742 A CN113912742 A CN 113912742A
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- carboxymethyl cellulose
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- 239000001768 carboxy methyl cellulose Substances 0.000 title claims abstract description 65
- 229920002134 Carboxymethyl cellulose Polymers 0.000 title claims abstract description 59
- 235000010948 carboxy methyl cellulose Nutrition 0.000 title claims abstract description 59
- 239000008112 carboxymethyl-cellulose Substances 0.000 title claims abstract description 59
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 55
- 238000006467 substitution reaction Methods 0.000 title claims abstract description 20
- 238000001308 synthesis method Methods 0.000 title description 3
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- AZVCGYPLLBEUNV-UHFFFAOYSA-N lithium;ethanolate Chemical compound [Li+].CC[O-] AZVCGYPLLBEUNV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 6
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 6
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 238000006138 lithiation reaction Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 230000020477 pH reduction Effects 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 2
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 abstract description 12
- 239000002994 raw material Substances 0.000 abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 8
- 239000002699 waste material Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 5
- 239000011230 binding agent Substances 0.000 abstract description 5
- 239000007863 gel particle Substances 0.000 abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 239000003513 alkali Substances 0.000 abstract description 4
- 229920002678 cellulose Polymers 0.000 abstract description 4
- 239000001913 cellulose Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000006182 cathode active material Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006257 cathode slurry Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B11/00—Preparation of cellulose ethers
- C08B11/02—Alkyl or cycloalkyl ethers
- C08B11/04—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
- C08B11/10—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals
- C08B11/12—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals substituted with carboxylic radicals, e.g. carboxymethylcellulose [CMC]
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method for synthesizing lithium carboxymethyl cellulose with ultrahigh substitution degree and ultrahigh viscosity, and relates to the technical field of lithium ion batteries. The invention comprises the following steps: acidifying, lithiating, washing, filtering, drying and crushing. According to the invention, the carboxymethyl cellulose lithium obtained through the steps does not directly use lithium hydroxide and ethanol as raw materials, the viscosity of the product is not reduced due to the alkali cellulose reaction at high temperature, the oxidation reaction of a high molecular chain at high temperature is avoided, and the aggravated oxidation fracture of the high molecular chain is avoided, so that the product has the advantages of high substitution degree and high viscosity, the process flow is simplified, the consumption of raw materials is effectively reduced, the lithium ethoxide is not required to be removed and can be recycled, the waste of materials is avoided, the generation of waste liquid is reduced, the production cost is reduced, the reaction is more thorough, the number of gel particles of the product is less, and the use effect of the carboxymethyl cellulose lithium as a lithium battery binder is more excellent.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a method for synthesizing carboxymethyl cellulose lithium with ultrahigh substitution degree and ultrahigh viscosity.
Background
Lithium carboxymethyl cellulose is frequently used as an aqueous thickener in the preparation of lithium ion battery cathodes, a cathode active material and a conductive agent are dispersed, the cathode active material and a current collector are bonded in an auxiliary manner, and the thickening effect is realized to prevent the cathode slurry from settling;
a specific processing method is required when the lithium carboxymethyl cellulose is produced;
the lithium carboxymethyl cellulose is a functional tackifier, has a tackifying effect in an aqueous system, and can provide lithium ions for the charge and discharge process;
after the graphite is adhered to the copper foil, the battery negative electrode is formed after drying, extruding and packaging, and the lithium ion is contained in the gap of the graphite system by adopting the carboxymethyl cellulose lithium as the tackifier, so that the resistance in the charging and discharging process is smaller, and the charging and discharging specific capacity and the multiplying power are larger;
in order to further improve the performance of lithium carboxymethyl cellulose, we propose a synthesis method of lithium carboxymethyl cellulose with ultrahigh substitution degree and ultrahigh viscosity, which has the following advantages:
1. lithium hydroxide and ethanol are not directly used as raw materials, the viscosity of the product is not reduced due to the alkali cellulose reaction at high temperature, the oxidation reaction of a high molecular chain at high temperature is avoided, and the aggravated oxidative fracture of the high molecular chain is avoided, so that the product has the advantages of high substitution degree and high viscosity;
2. the process flow is simplified, and the consumption of raw materials is effectively reduced;
3. the lithium ethylate can be recycled without being removed, so that the waste of materials is avoided, the generation of waste liquid is reduced, the production cost is reduced, the reaction is more thorough, the number of gel particles of the product is less, and the using effect of the lithium ethylate serving as a lithium battery binder is more excellent.
Disclosure of Invention
The invention aims to provide a method for synthesizing lithium carboxymethyl cellulose with ultrahigh substitution degree and ultrahigh viscosity, which can effectively improve the substitution degree and viscosity of the lithium carboxymethyl cellulose, simplify the process flow, reduce the consumption of raw materials, reduce the production cost, ensure more thorough reaction, reduce the number of gel particles of a product and have more excellent use effect as a lithium battery binder.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a method for synthesizing carboxymethyl cellulose lithium with ultrahigh substitution degree and ultrahigh viscosity, which comprises the following steps:
acidifying, namely adding acid into the sodium carboxymethyl cellulose for acidification reaction to generate carboxymethyl cellulose hydrogen;
lithiation, namely adding lithium ethoxide into carboxymethyl cellulose hydrogen, and carrying out chemical reaction at the temperature of 55-65 ℃ to generate the carboxymethyl cellulose lithium.
Further, the method also comprises the following steps:
washing, namely alternately and repeatedly washing the carboxymethyl cellulose lithium by using ionized water and methanol until the generated carboxymethyl cellulose lithium is neutral;
filtering water, namely filtering the lithium carboxymethyl cellulose to filter liquid in the lithium carboxymethyl cellulose;
drying, namely drying the lithium carboxymethyl cellulose;
and (3) crushing, namely crushing the lithium carboxymethyl cellulose by using a crushing machine until the lithium carboxymethyl cellulose is in a powder shape.
Further, the sodium carboxymethylcellulose and acid are mixed according to a ratio of 1: 0.2-0.35 in proportion.
Further, the acid is one or more of dilute acid, concentrated acid, such as acetic acid, hydrochloric acid, sulfuric acid, and nitric acid.
Further, the carboxymethyl cellulose hydrogen and lithium ethoxide are mixed according to a ratio of 1: 0.1 to 1.0 in proportion.
Further, the drying temperature is 60-80 ℃.
The invention has the following beneficial effects:
according to the invention, the carboxymethyl cellulose lithium obtained through the steps does not directly use lithium hydroxide and ethanol as raw materials, the viscosity of the product is not reduced due to the alkali cellulose reaction at high temperature, the oxidation reaction of a high molecular chain at high temperature is avoided, and the aggravated oxidation fracture of the high molecular chain is avoided, so that the product has the advantages of high substitution degree and high viscosity, the process flow is simplified, the consumption of raw materials is effectively reduced, the lithium ethoxide is not required to be removed and can be recycled, the waste of materials is avoided, the generation of waste liquid is reduced, the production cost is reduced, the reaction is more thorough, the number of gel particles of the product is less, and the use effect of the carboxymethyl cellulose lithium as a lithium battery binder is more excellent.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a reaction diagram of a method for synthesizing lithium carboxymethyl cellulose with ultra-high degree of substitution and ultra-high viscosity according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention is a method for synthesizing lithium carboxymethyl cellulose with ultra-high degree of substitution and ultra-high viscosity, comprising the following steps:
s1, acidifying, namely adding acid into the sodium carboxymethyl cellulose to carry out acidification reaction to generate carboxymethyl cellulose hydrogen;
here, the sodium carboxymethylcellulose and the acid are mixed in a ratio of 1: 0.2-0.35;
the acid is one or more of dilute acid, concentrated acid, such as acetic acid, hydrochloric acid, sulfuric acid and nitric acid;
s2, lithiation, namely adding lithium ethoxide into carboxymethyl cellulose hydrogen, and carrying out chemical reaction at the temperature of 55-65 ℃ to generate the carboxymethyl cellulose lithium;
here, the carboxymethyl cellulose hydrogen and lithium ethoxide were mixed in a ratio of 1: the ratio of 0.1-1.0;
s3, washing, namely, alternately and repeatedly washing the lithium carboxymethyl cellulose by using ionized water and methanol until the generated lithium carboxymethyl cellulose is neutral;
s4, filtering water, namely filtering the lithium carboxymethyl cellulose, and filtering liquid in the lithium carboxymethyl cellulose;
s5, drying, namely drying the lithium carboxymethyl cellulose at the drying temperature of 60-80 ℃;
s6, crushing, namely crushing the lithium carboxymethyl cellulose by using a crushing machine until the lithium carboxymethyl cellulose is powdery;
in conclusion, the carboxymethyl cellulose lithium obtained through the steps of the invention does not directly use lithium hydroxide and ethanol as raw materials, does not reduce the viscosity of the product due to the alkali cellulose reaction at high temperature, has the advantages of high substitution degree and high viscosity, simplifies the process flow, effectively reduces the consumption of raw materials, can be recycled without removing the lithium ethoxide, avoids the waste of materials, reduces the generation of waste liquid, reduces the production cost, has more thorough reaction, has fewer gel particles of the product, and has more excellent use effect as a lithium battery binder.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (6)
1. A method for synthesizing lithium carboxymethyl cellulose with ultrahigh substitution degree and ultrahigh viscosity comprises the following steps:
acidifying, namely adding acid into the sodium carboxymethyl cellulose for acidification reaction to generate carboxymethyl cellulose hydrogen;
lithiation, namely adding lithium ethoxide into carboxymethyl cellulose hydrogen, and carrying out chemical reaction at the temperature of 55-65 ℃ to generate the carboxymethyl cellulose lithium.
2. The method for synthesizing lithium carboxymethyl cellulose with ultrahigh degree of substitution and ultrahigh viscosity according to claim 1, further comprising the steps of:
washing, namely alternately and repeatedly washing the carboxymethyl cellulose lithium by using ionized water and methanol until the generated carboxymethyl cellulose lithium is neutral;
filtering water, namely filtering the lithium carboxymethyl cellulose to filter liquid in the lithium carboxymethyl cellulose;
drying, namely drying the lithium carboxymethyl cellulose;
and (3) crushing, namely crushing the lithium carboxymethyl cellulose by using a crushing machine until the lithium carboxymethyl cellulose is in a powder shape.
3. The method for synthesizing lithium carboxymethyl cellulose with ultrahigh degree of substitution and ultrahigh viscosity according to claim 1, wherein the ratio of sodium carboxymethyl cellulose to acid is 1: 0.2-0.35 in proportion.
4. The method for synthesizing lithium carboxymethyl cellulose with ultrahigh degree of substitution and ultrahigh viscosity according to claim 1, wherein the acid is one or more of diluted acid, concentrated acid, such as acetic acid, hydrochloric acid, sulfuric acid and nitric acid.
5. The method for synthesizing lithium carboxymethyl cellulose with ultrahigh substitution degree and ultrahigh viscosity according to claim 1, wherein the ratio of carboxymethyl cellulose hydrogen to lithium ethoxide is 1: 0.1 to 1.0 in proportion.
6. The method for synthesizing lithium carboxymethyl cellulose with ultrahigh substitution degree and ultrahigh viscosity according to claim 2, wherein the drying temperature is 60-80 ℃.
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| CN202111041757.1A CN113912742A (en) | 2021-09-07 | 2021-09-07 | Synthesis method of lithium carboxymethyl cellulose with ultrahigh substitution degree and ultrahigh viscosity |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805614A (en) * | 2022-05-18 | 2022-07-29 | 向能新型材料科技(河北)有限公司 | Preparation method of lithium sulfomethyl cellulose as lithium battery binder |
| CN115043949A (en) * | 2022-07-26 | 2022-09-13 | 绿能纤材(重庆)科技有限公司 | Synthesis method of low-gel particle high-transparency carboxymethyl cellulose lithium aqueous binder |
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| US20160102153A1 (en) * | 2013-06-04 | 2016-04-14 | Dow Global Technologies Llc | Process for manufacturing lithium carboxymethyl cellulose |
| CN112724266A (en) * | 2020-12-28 | 2021-04-30 | 常熟威怡科技有限公司 | Preparation method of lithium carboxymethyl cellulose for lithium battery |
| CN113265008A (en) * | 2021-07-02 | 2021-08-17 | 重庆力宏精细化工有限公司 | High-viscosity lithium carboxymethyl cellulose and preparation method and application thereof |
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2021
- 2021-09-07 CN CN202111041757.1A patent/CN113912742A/en active Pending
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| US20160102153A1 (en) * | 2013-06-04 | 2016-04-14 | Dow Global Technologies Llc | Process for manufacturing lithium carboxymethyl cellulose |
| CN112724266A (en) * | 2020-12-28 | 2021-04-30 | 常熟威怡科技有限公司 | Preparation method of lithium carboxymethyl cellulose for lithium battery |
| CN113265008A (en) * | 2021-07-02 | 2021-08-17 | 重庆力宏精细化工有限公司 | High-viscosity lithium carboxymethyl cellulose and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805614A (en) * | 2022-05-18 | 2022-07-29 | 向能新型材料科技(河北)有限公司 | Preparation method of lithium sulfomethyl cellulose as lithium battery binder |
| CN115043949A (en) * | 2022-07-26 | 2022-09-13 | 绿能纤材(重庆)科技有限公司 | Synthesis method of low-gel particle high-transparency carboxymethyl cellulose lithium aqueous binder |
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