CN109638286B - Carboxymethyl cellulose-based binder and application thereof in lithium battery - Google Patents
Carboxymethyl cellulose-based binder and application thereof in lithium battery Download PDFInfo
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- CN109638286B CN109638286B CN201811446063.4A CN201811446063A CN109638286B CN 109638286 B CN109638286 B CN 109638286B CN 201811446063 A CN201811446063 A CN 201811446063A CN 109638286 B CN109638286 B CN 109638286B
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- 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
- H01M4/622—Binders being polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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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Abstract
The invention relates to a carboxymethyl cellulose-based binder, which comprises the following components in parts by weight: 30-40 parts of sodium carboxymethylcellulose, 10-20 parts of modified SBR, 1-5 parts of tea saponin, 1-5 parts of a thickening agent and 5-10 parts of a diluting auxiliary agent; the binder prepared by the method has the advantages of finer particle size and good intersolubility with each component, so that the surface defect of the pole piece is almost zero, the flexibility of a binder system can be improved, and the problem of pole piece cracking is solved.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a carboxymethyl cellulose-based binder and application thereof in a lithium battery.
Background
In recent years, with the further landing and promotion of national new energy policies, the new energy automobile industry has been developed greatly. But the market demand for battery products with high energy density and high specific power is therefore more and more urgent. The development of lithium ion electrode materials and related auxiliary materials with high specific energy and low cost is becoming the research and development focus of various large battery core manufacturers and material suppliers. Under the development trend of high energy density, the material systems of anode and cathode materials, diaphragms, electrolytes and the like of the current lithium ion power battery are continuously upgraded. In addition to these main raw materials, auxiliary materials, which are used in very small amounts but are nevertheless of critical importance, have also been revolutionized in the performance of products, for example lithium battery binders.
Currently, polyvinylidene fluoride (PVDF) is generally used as a binder in the large-scale production of lithium ion batteries, and is expensive, and an explosive and environmentally unfriendly organic solvent such as N-methylpyrrolidone (NMP) is also required to be used in the application process, so that the requirement on the air humidity of the production process is strict, secondary reaction with metal lithium and lithium intercalation graphite is easy to occur, and particularly, the risk of spontaneous heating runaway exists at a high temperature. The water-soluble binder-sodium carboxymethylcellulose is used as a substitute of PVDF for an electrode material, so that the use of NMP can be avoided, the cost is reduced, and the environmental pollution is reduced; meanwhile, the production process has no requirement on the environment humidity, the capacity of the battery can be improved, and the cycle life is prolonged.
The Chinese patent with the application publication number of CN107910556A in the prior patent discloses a lithium battery anode material and a preparation method thereof, wherein the lithium battery anode material is composed of the following raw materials in parts by weight: 100-110 parts of lithium hydroxide, 20-30 parts of manganese sulfate, 4-6 parts of cobaltous oxide, 2-3 parts of conductive adhesive liquid, 7-9 parts of zinc oxide, 0.1-0.2 part of sodium carboxymethylcellulose and 0.08-0.1 part of stannous sulfate.
However, when the sodium carboxymethylcellulose in the prior art is mixed with a plurality of components, larger particles exist in a mixing system, which affects the softness of the pole piece and increases the surface defects of the pole piece.
Disclosure of Invention
The invention aims to provide a carboxymethyl cellulose-based binder which has fine particles, can improve the flexibility of a pole piece and reduce the surface defects of the pole piece.
The above object of the present invention is achieved by the following technical solutions:
the carboxymethyl cellulose-based binder comprises the following components in parts by weight: 30-40 parts of sodium carboxymethylcellulose, 10-20 parts of modified SBR, 1-5 parts of tea saponin, 1-5 parts of a thickening agent and 5-10 parts of a diluting auxiliary agent.
By adopting the technical scheme, the sodium carboxymethylcellulose (CMC-Na) is cellulose which has the widest application range and the largest using amount in the world at present, is a cellulose derivative with the glucose polymerization degree of 100-2000, has relative molecular mass of 242.16, is white fibrous or granular powder, is odorless, tasteless, hygroscopic and insoluble in organic solvents; the sodium carboxymethyl cellulose can also improve the sedimentation of a slurry system; the particle size is fine, the compatibility with other components is good, and insoluble substances are almost eliminated; the SBR latex particle unit is a core-shell structure, a cross-linked structure of a copolymer molecular chain is arranged in the shell, the outer shell is a hydrophilic polar group and a surfactant, and a water-based group in the SBR is combined with an aluminum foil base material to form a binding force, so that the dispersibility and the slurry stability are facilitated; the oily group is combined with the negative electrode material to form binding power, so that a binding effect is achieved; however, SBR is easy to be oxidized at high potential, meanwhile, the dispersibility of SBR in an electrode system is not good, the modified SBR has good dispersibility and stable performance, and is not easy to be oxidized at high potential, and the viscosity of the system is reduced in the processing process of the modified SBR, so that roll sticking is prevented during tabletting; the tea saponin is a glucoside compound extracted from tea tree seeds, is a natural surfactant with good performance, and is beneficial to improving the compatibility and permeability among various components and inhibiting the decomposition performance of CMC-Na at high temperature; the thickening agent can improve the viscosity degree of the system, and can flexibly adjust the viscosity in the system according to different requirements; the diluting auxiliary agent improves the compatibility among all components, enhances the permeability of the sodium carboxymethylcellulose, better mixes and dissolves with other components, the particle size of the binding agent prepared by the method is thinner, the intersolubility with all the components is good, the surface defect of the pole piece is almost zero, the flexibility of a binding agent system can be improved, and the problem of pole piece cracking is solved.
The invention is further configured to: the substitution degree of the sodium carboxymethyl cellulose is 0.5-0.8.
By adopting the technical scheme, the CMC-Na in the substitution degree range is in a granular structure, has a stable structure, reduces the agglomeration of the CMC-Na and other components, obviously reduces the grain size of a binder system, and is beneficial to the exertion of electrochemical performance.
The invention is further configured to: the modified SBR is formed by carrying out hydrophobic treatment on SBR to form SBR-SiO2And (4) mucilage.
By adopting the technical scheme, SiO is utilized2The SBR is subjected to hydrophobic treatment, so that the surface of the SBR is rougher, a low-surface-energy substance is introduced to prepare a hydrophobic coating, and the SBR formed by hydrophobic modification is doped in a pole piece system, so that the phenomenon of roller sticking during sheet making can be effectively prevented.
The invention is further configured to: the thickening agent comprises the following components in parts by weight: 30-40 parts of acrylates, 5-20 parts of carboxymethyl starch ether, 3-10 parts of carbomer, 3-10 parts of xanthan gum and 1-5 parts of POSS.
By adopting the technical scheme, a certain amount of carboxyl is introduced into starch molecules by the carboxymethyl starch ether, so that the carboxymethyl starch has larger molecular weight than common starch, shows inherent properties of the carboxyl such as hydrophilicity, complexation and the like, and can be suitable for various industries such as thickening agents, stabilizing agents, film forming agents, flocculating agents, adhesives and the like; the acrylic ester, the carboxymethyl starch ether, the carbomer, the xanthan gum and the POSS are blended, so that the obtained thickener has good leveling property, is beneficial to seeping into other components in a system, and can widen the particle size range of the system besides adjusting the viscosity of a binder system.
The invention is further configured to: the viscosity of the thickening agent is 1000-5000 mpa for seconds.
By adopting the technical scheme, the viscosity range of the thickening agent is wider, and the application range of the product is improved.
The invention is further configured to: the diluting auxiliary agent comprises the following components in parts by weight: 1-5 parts of alpha-sodium alkenyl sulfonate, 1.5-3 parts of isomeric alcohol polyoxyethylene ether and 3-5 parts of JFC penetrant.
By adopting the technical scheme, the alpha-sodium alkenyl sulfonate has excellent surface activity, and the surface tension of water is obviously reduced within a certain concentration range; accordingly, the water-soluble calcium soap has excellent solubility, wettability, foamability, hard water resistance and calcium soap dispersivity; has good detergency, and particularly shows the characteristic of no reduction of the detergency in hard water; in addition, the biodegradable polyester has good biodegradability; the isomeric alcohol polyoxyethylene ether is colorless or light yellow liquid, is easy to dissolve in water, has excellent emulsification, cleaning and detergency and hard water resistance, has good chemical stability and environmental compatibility in a wider pH value range, and can be used as a dispersant, a wetting agent, a penetrant and a detergent; the JFC penetrant is a liquid material with extremely strong permeability, has good adhesive force, is quick to dry and strong in wear resistance, and also has good chemical resistance and water resistance; the alpha-sodium alkenyl sulfonate, the isomeric alcohol polyoxyethylene ether and the JFC penetrant are blended, so that the mutual solubility of all components in a system is improved.
The invention is further configured to: the adhesive is prepared by the following steps:
(1) weighing;
(2) permeating the diluting auxiliary agent into the sodium carboxymethylcellulose, and keeping for at least 30min to obtain a premix;
(3) then adding the modified SBR and the tea saponin into the premix, and stirring at a high speed for 2-3 h;
(4) and continuously adding the thickening agent, and stirring for 0.5-1 h.
By adopting the technical scheme, the binder is prepared by adopting the formula, the diluting auxiliary agent is added into the sodium carboxymethyl cellulose in advance to improve the intersolubility of the sodium carboxymethyl cellulose and other components, and then the sodium carboxymethyl cellulose is blended with the modified SBR and the tea saponin again to further improve the fineness of a binder system.
The second aim of the invention is realized by the following technical scheme:
the application of carboxymethyl cellulose-based binder is applicable to the processing field of manufacturing lithium batteries.
By adopting the technical scheme, the adhesive is prepared according to the formula, and the adhesive is applied to the field of lithium batteries, so that the quality of the pole piece can be obviously improved.
In conclusion, the beneficial technical effects of the invention are as follows:
1. discloses a novel carboxymethyl cellulose-based binder, the binder system has fine particles, and can improve the flexibility of a pole piece and reduce the surface defects of the pole piece;
2. the binder takes sodium carboxymethylcellulose as a main body, is doped with the modified SBR, has good dispersibility and stable performance, is not easy to oxidize under high potential, reduces the viscosity of a system in the processing process of the modified SBR, and prevents roll sticking in tabletting;
3. the application is to permeate the diluting auxiliary agent into the sodium carboxymethyl cellulose, so that the miscibility of the sodium carboxymethyl cellulose and other components is favorably improved, and the fineness uniformity of a binder system is improved.
Detailed Description
The present invention will be described in further detail with reference to examples.
Preparation work:
firstly, modified SBR is prepared by the following steps:
(1) dripping 3-5 drops of hydroxyl silicone oil into 30-40 parts of SBR according to parts by weight, diluting the SBR, and keeping permeation for 30 min;
(2) continuously adding 5-10 parts of SiO2Then, the mixture is stirred at a high speed to form a viscous colloid.
Secondly, the thickener is prepared by the following steps:
(1) preparing materials: weighing 30-40 parts of acrylate, 5-20 parts of carboxymethyl starch ether, 3-10 parts of carbomer, 3-10 parts of xanthan gum and 1-5 parts of POSS (polyhedral oligomeric silsesquioxane);
(2) adding carboxymethyl starch ether into the acrylic ester, adjusting the rotating speed to 150r/min, and stirring for 1-1.5 h;
(3) and continuously adding POSS, carbomer and xanthan gum, and increasing the rotating speed to 200-220 r/min to obtain the thickening agent.
Thirdly, diluting the auxiliary agent, and preparing by adopting the following steps:
(1) preparing materials: weighing 1-5 parts of alpha-sodium alkenyl sulfonate, 1.5-3 parts of isomeric alcohol polyoxyethylene ether and 3-5 parts of JFC penetrant;
(2) adding the alpha-sodium alkenyl sulfonate, the isomeric alcohol polyoxyethylene ether and the JFC penetrant into a stirring tank, and adjusting the stirring speed to be 100r/min to obtain the diluting auxiliary agent.
The first embodiment is as follows:
(1) preparing materials: 30 parts of sodium carboxymethylcellulose, 10 parts of modified SBR, 1 part of tea saponin, 1 part of thickener and 5 parts of diluting auxiliary agent;
(2) permeating the diluting auxiliary agent into the sodium carboxymethylcellulose, and keeping for at least 30min to obtain a premix;
(3) then adding the modified SBR and the tea saponin into the premix, and stirring at a high speed for 2-3 h;
(4) and continuously adding the thickening agent, and stirring for 0.5-1 h.
Example two:
(1) preparing materials: 32 parts of sodium carboxymethylcellulose, 12 parts of modified SBR, 2 parts of tea saponin, 2 parts of a thickening agent and 6 parts of a diluting auxiliary agent;
(2) permeating the diluting auxiliary agent into the sodium carboxymethylcellulose, and keeping for at least 30min to obtain a premix;
(3) then adding the modified SBR and the tea saponin into the premix, and stirring at a high speed for 2-3 h;
(4) and continuously adding the thickening agent, and stirring for 0.5-1 h.
Example three:
(1) preparing materials: 34 parts of sodium carboxymethylcellulose, 14 parts of modified SBR, 3 parts of tea saponin, 3 parts of a thickening agent and 7 parts of a diluting auxiliary agent;
(2) permeating the diluting auxiliary agent into the sodium carboxymethylcellulose, and keeping for at least 30min to obtain a premix;
(3) then adding the modified SBR and the tea saponin into the premix, and stirring at a high speed for 2-3 h;
(4) and continuously adding the thickening agent, and stirring for 0.5-1 h.
Example four:
(1) preparing materials: 38 parts of sodium carboxymethylcellulose, 18 parts of modified SBR, 4 parts of tea saponin, 4 parts of a thickening agent and 9 parts of a diluting auxiliary agent;
(2) permeating the diluting auxiliary agent into the sodium carboxymethylcellulose, and keeping for at least 30min to obtain a premix;
(3) then adding the modified SBR and the tea saponin into the premix, and stirring at a high speed for 2-3 h;
(4) and continuously adding the thickening agent, and stirring for 0.5-1 h.
Example five:
(1) preparing materials: 40 parts of sodium carboxymethylcellulose, 20 parts of modified SBR, 5 parts of tea saponin, 5 parts of a thickening agent and 10 parts of a diluting auxiliary agent;
(2) permeating the diluting auxiliary agent into the sodium carboxymethylcellulose, and keeping for at least 30min to obtain a premix;
(3) then adding the modified SBR and the tea saponin into the premix, and stirring at a high speed for 2-3 h;
(4) and continuously adding the thickening agent, and stirring for 0.5-1 h.
Comparative example: the prior patent application publication No. CN107910556A was used as a comparative example.
The detection method comprises the following steps:
(1) flexibility: and folding the pole piece for three times, and then detecting the energy density.
(2) And (3) surface defect detection: the defects of the pole pieces are detected by adopting the visual inspection developed by the creative and new technology company.
The results of the flexibility test are shown in the following table:
| sample (I) | Specific discharge capacity (mAh/g) | Specific discharge capacity (mAh/g) after 100 charge-discharge cycles |
| Example one | 1560 | 1420 |
| Example two | 1580 | 1430 |
| EXAMPLE III | 1590 | 1450 |
| Example four | 1600 | 1460 |
| EXAMPLE five | 1580 | 1450 |
| Comparative example | 870 | 0 |
As can be seen from the above table, after three times of folding, the comparative sample is broken and cannot be conducted, and each sample in the embodiment can be conducted, and still can emit more specific capacity, and has good flexibility and excellent cycle performance.
The results of the surface defect measurements are shown in the following table:
| sample (I) | Surface condition of the surface |
| Example one | Defect free |
| Example two | Defect free |
| EXAMPLE III | Defect free |
| Example four | Defect free |
| EXAMPLE five | Defect free |
| Comparative example | Material dropping; with a pinhole |
According to the table, in the embodiment, each sample has good surface quality, so that the particles of the components are fine and uniform, and the pole piece prepared by the comparative example method has serious surface defects, high defective rate and short service life, and is not beneficial to large-scale production.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (3)
1. The carboxymethyl cellulose-based binder is characterized by comprising the following components in parts by weight: 30-40 parts of sodium carboxymethylcellulose, 10-20 parts of modified SBR, 1-5 parts of tea saponin, 1-5 parts of a thickening agent and 5-10 parts of a diluting auxiliary agent, wherein the substitution degree of the sodium carboxymethylcellulose is 0.5-0.8;
the thickener is prepared by the following steps: (1) preparing materials: weighing 30-40 parts of acrylate, 5-20 parts of carboxymethyl starch ether, 3-10 parts of carbomer, 3-10 parts of xanthan gum and 1-5 parts of POSS (polyhedral oligomeric silsesquioxane); (2) adding carboxymethyl starch ether into the acrylic ester, adjusting the rotating speed to 150r/min, and stirring for 1-1.5 h; (3) and continuously adding POSS, carbomer and xanthan gum, and increasing the rotating speed to 200-220 r/min to obtain the thickening agent.
2. The carboxymethyl cellulose-based binder according to claim 1, comprising the following components in parts by weight: 38 parts of sodium carboxymethylcellulose, 18 parts of modified SBR, 4 parts of tea saponin, 4 parts of a thickening agent and 9 parts of a diluting auxiliary agent.
3. The carboxymethyl cellulose-based binder according to claim 1, which is prepared by the steps of:
(1) weighing;
(2) permeating the diluting auxiliary agent into the sodium carboxymethylcellulose, and keeping for at least 30min to obtain a premix;
(3) then adding the modified SBR and the tea saponin into the premix, and stirring at a high speed for 2-3 h;
(4) and continuously adding the thickening agent, and stirring for 0.5-1 h.
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| CN112803000A (en) * | 2019-11-14 | 2021-05-14 | 孚能科技(赣州)股份有限公司 | Composition for battery negative plate coating, battery negative plate coating slurry, and preparation method and application thereof |
| CN111900393A (en) * | 2020-06-24 | 2020-11-06 | 珠海冠宇电池股份有限公司 | High-ionic-conductivity binder and lithium ion battery containing same |
| CN113088232B (en) * | 2021-05-14 | 2023-04-18 | 河北星辰工程科技有限公司 | Slow-bonding agent and slow-bonding prestressed steel bar |
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