CN114409841A - Emulsion polymerization high-molecular dispersing agent for replacing CMC (carboxy methyl cellulose) of lithium battery and preparation method thereof - Google Patents
Emulsion polymerization high-molecular dispersing agent for replacing CMC (carboxy methyl cellulose) of lithium battery and preparation method thereof Download PDFInfo
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F218/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
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- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
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- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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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
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Abstract
The invention discloses an emulsion polymerization macromolecular dispersant for replacing CMC (carboxy methyl cellulose) of a lithium battery, which mainly comprises unsaturated monomers, water, an emulsifier and a water-soluble initiator, wherein the emulsion polymerization is prepared by polymerizing various unsaturated monomers and water in emulsion prepared under the action of the emulsifier, and the unsaturated monomers comprise but are not limited to: one or more of acrylic acid, methacrylic acid, methyl methacrylate, styrene, vinyl acetate, butyl acrylate, isooctyl acrylate, acrylamide and N-methyl acrylamide, and the main chain of the macromolecular dispersant is a-C-C-bond. The invention uses a simple and environment-friendly method to obtain the polymer dispersant which can be designed on the main chain of a polymer framework in advance, is more excellent than CMC and is more suitable for lithium batteries, and can improve the performance of the existing lithium batteries to replace the CMC dispersant widely used at present.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to an emulsion polymerization high polymer dispersant for replacing CMC (carboxy methyl cellulose) by a lithium battery.
Background
The traditional lithium battery negative electrode slurry uses CMC-carboxymethyl cellulose as a dispersing agent, and the production method thereof is approximately as follows: soaking the degreased and bleached cotton threads into 35% of concentrated alkali liquor in proportion, and taking out after soaking for about 30 min. Liquid alkali can be recycled, the soaked cotton is weighed on a flat-plate squeezer in short line, alkali liquor is pressed out under the pressure of 14 MPa to obtain alkalized cotton, the alkalized cotton is put into an etherification kettle, 15 parts of alcohol is added into chloroacetic acid alcohol solution slowly under stirring, the mixture is stirred for 2 hours at the temperature of 30 ℃, the mixture is stirred for 3 hours at the temperature of 40 ℃ after the alkali solution is added, 120 parts of alcohol (70%) is added into the etherified cotton, the mixture is stirred for 0.5 hour, hydrochloric acid is added to adjust the pH value to 7, the mixture is washed twice by alcohol, the alcohol is filtered out, air blowing drying is carried out at the temperature of 80 ℃, the mixture is crushed to obtain a finished product, and low-substitution degree (less than 0.4) and medium-substitution degree (0.4-1.2) products can be produced according to different mixture ratios, and the CMC structure and the production process can be seen from the above: CMC is prepared by using natural substances as a base material through chemical modification, a main chain framework is fixed, the optimization of large performance is not easy, the production process of the CMC dispersant is complex, strong acid and strong alkali are used, the risk of chemical corrosion and burn is high, the three wastes are generated, the influence on the environment is large, and more impurities possibly remained in the product are generated.
Therefore, we propose an emulsion polymerization polymer dispersant for replacing CMC in lithium battery to solve the above problems.
Disclosure of Invention
The invention aims to provide an emulsion polymerization polymer dispersant for replacing CMC (carboxy methyl cellulose) for a lithium battery, which can be designed on a main chain of a polymer framework in advance by a simple and environment-friendly method, has more excellent performance than CMC and is more suitable for the lithium battery, and can improve the performance of the conventional lithium battery to replace the CMC dispersant widely used at present so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
an emulsion polymerization high molecular dispersant for replacing CMC (carboxy methyl cellulose) of a lithium battery mainly comprises unsaturated monomers, water, an emulsifier and a water-soluble initiator, wherein the emulsion polymerization is prepared by polymerizing various unsaturated monomers and water in an emulsion prepared by the action of the emulsifier, and the unsaturated monomers include but are not limited to: one or more of acrylic acid, methacrylic acid, methyl methacrylate, styrene, vinyl acetate, butyl acrylate, isooctyl acrylate, acrylamide and N-methyl acrylamide, and the main chain of the macromolecular dispersant is a-C-C-bond.
A preparation process of an emulsion polymerization macromolecular dispersant for replacing CMC (carboxyl methyl cellulose) of a lithium battery comprises the steps of A, material preparation, B, heating and dissolving, C, synthesis reaction, D, cooling, E, packaging and discharging.
In a further embodiment, the a. stock: the liquid raw materials are automatically weighed and fed, and the solid raw materials are manually fed. The method comprises three parts: firstly, pumping monomer vinyl acetate, butyl acrylate, isooctyl acrylate and other monomer materials into a pre-emulsification kettle, starting stirring for pre-emulsification to obtain pre-emulsion, secondly, adding an initiator and process water into the initiator kettle, uniformly stirring, thirdly, adding an emulsifier, process water and the like into a polymerization kettle, and uniformly stirring.
In a further embodiment, the b. Heating the polymerization kettle to 80-86 ℃, preserving heat for 10-30 minutes, and stirring and mixing uniformly.
In a further embodiment, the c. synthesis reaction: and dropwise adding a small amount of pre-emulsion into a polymerization kettle from a pre-emulsion kettle, continuously heating, adding a priming initiator when the temperature is raised to 78-84 ℃, and carrying out a priming reaction. After the bottoming reaction is finished, the pre-emulsion is dripped to carry out synthetic reaction, the temperature is controlled to be 80-86 ℃, the time is about 4-6 hours, and cooling water is added into a jacket of a reaction kettle to control the reaction temperature to be 80-86 ℃ along with the reaction.
In a further embodiment, the d. After the polymerization reaction is finished, the temperature in the kettle is reduced to below 50 ℃ through the heat preservation process and the cooling, and the post-treatment agent is added for adjustment.
Compared with the prior art, the invention has the beneficial effects that:
the invention uses a simple and environment-friendly method to obtain a macromolecular dispersant which can be designed on a macromolecular skeleton main chain in advance, is more excellent than CMC and is more suitable for lithium batteries, can improve the performance of the existing lithium batteries to replace the CMC dispersant widely used at present, adopts normal-temperature monomers, an emulsifier and water to be mixed and pre-emulsified, then bottoming to initiate polymerization, slowly dripping at constant temperature of 80 ℃ to maintain the completion of polymerization reaction, preserving heat and eliminating residues to ensure complete reaction, then cooling and adding a post-treatment agent, and simply for 8-10 hours to complete the whole production process, finally all additives become the macromolecular dispersant product, and the macromolecular dispersant product can be directly used for lithium battery production without generating any by-product to reduce the waste of resources and the influence on the environment. The used medium is water, the method is safe, environment-friendly and economical, a chemical synthesis method is used for replacing a bio-based structure, the main chain of a macromolecule is similar to the structure of CMC and is superior to the structure of CMC, so that the dispersion is very good, the adhesive property, the conductivity and the high and low temperature are excellent, and the composition of a formula and the structure of the main chain are protected. 2. The special emulsion polymerization method is adopted, and the molecular weight of the obtained polymer is large and is 100-200 ten thousand, so that the polymer has good performances in all aspects.
Drawings
FIG. 1 is a schematic diagram of a specific reaction equation of an emulsion polymerization polymeric dispersant;
FIG. 2 is a process flow diagram of emulsion polymerization polymeric dispersant.
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.
The emulsion polymerization high-molecular dispersing agent for replacing CMC (carboxyl methyl cellulose) of the lithium battery mainly comprises unsaturated monomers, water, an emulsifier and a water-soluble initiator, wherein the emulsion polymerization is prepared by polymerizing various unsaturated monomers and water in an emulsion prepared by the action of the emulsifier, and the unsaturated monomers comprise but are not limited to: one or more of acrylic acid, methacrylic acid, methyl methacrylate, styrene, vinyl acetate, butyl acrylate, isooctyl acrylate, acrylamide and N-methyl acrylamide, and the main chain of the macromolecular dispersant is a-C-C-bond.
The emulsion polymerization comprises the following steps: various unsaturated monomers (including but not limited to acrylic acid, methacrylic acid, methyl methacrylate, styrene, vinyl acetate, butyl acrylate, isooctyl acrylate, acrylamide, N-methyl acrylamide and the like), an emulsifier and an initiator carry out high-molecular polymerization reaction at about 80 ℃ by using water as a medium and a carrier according to a certain process sequence process to obtain the high-molecular dispersing agent with the desired performance. The reaction condition is mild, the reaction temperature is 80 ℃, strong corrosivity of strong acid and alkali is avoided, all materials are subjected to reaction and post-treatment after being put into the reaction kettle and are reserved in the product to become useful components, the useful components are directly used for the lithium battery, no useless by-products are generated, the environment is not affected, and the used medium is water, so that the reaction kettle is safe, low-carbon, environment-friendly and economical.
The specific reaction scheme is schematically shown in FIG. 1 (three unsaturated monomers are only schematic to include the above-mentioned plural).
The technological process is a semi-continuous process and comprises the steps of material preparation, heating dissolution, synthesis reaction, cooling, adjustment, detection, filtration, packaging and the like; the production process needs 8-10 h:
A. preparing materials: the liquid raw materials are automatically weighed and fed, and the solid raw materials are manually fed. The method comprises three parts: firstly, pumping monomer vinyl acetate, butyl acrylate, isooctyl acrylate and other monomer materials into a pre-emulsification kettle, starting stirring for pre-emulsification to obtain pre-emulsion, secondly, adding an initiator and process water into the initiator kettle, uniformly stirring, thirdly, adding an emulsifier, the process water and the like into a polymerization kettle, and uniformly stirring;
B. heating for dissolving: heating the polymerization kettle to 80-86 ℃, preserving heat for 10-30 minutes, and stirring and mixing uniformly;
C. and (3) synthesis reaction: and dropwise adding a small amount of pre-emulsion into a polymerization kettle from a pre-emulsion kettle, continuously heating, adding a priming initiator when the temperature is raised to 78-84 ℃, and carrying out a priming reaction. After the bottoming reaction is finished, starting to dropwise add the pre-emulsion to perform a synthesis reaction, controlling the temperature to be 80-86 ℃, wherein the time is about 4-6 hours, and adding cooling water into a reaction kettle jacket to control the reaction temperature to be 80-86 ℃ along with the reaction;
D. and (3) cooling: after the polymerization reaction is finished, the temperature in the kettle is reduced to below 50 ℃ through the heat preservation process and the cooling, and post-treatment agents and the like are added for adjustment;
E. packaging and discharging: after the adjustment, the product is qualified by inspection, filtered, packaged and discharged.
The process flow is shown in figure 2.
The invention replaces the structure of biology base with chemical synthesis method, the main chain of macromolecule is similar to the structure of CMC, but is superior to the structure of CMC, so that it has very good dispersivity, and also has excellent cohesiveness, conductivity, high and low temperature, and we want to protect the composition of formula and the structure of main chain. 2. The special emulsion polymerization method is adopted, and the molecular weight of the obtained polymer is large and is 100-200 ten thousand, so that the polymer has good performances in all aspects.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. An emulsion polymerization macromolecular dispersant for lithium battery CMC, which is characterized in that: the emulsion polymerization is prepared by polymerizing various unsaturated monomers and water in emulsion prepared by the unsaturated monomers and the water under the action of the emulsifier; the unsaturated monomers include, but are not limited to: one or more of acrylic acid, methacrylic acid, methyl methacrylate, styrene, vinyl acetate, butyl acrylate, isooctyl acrylate, acrylamide, and N-methyl acrylamide; the main chain of the macromolecular dispersant is a-C-C-bond.
2. The preparation process of the emulsion polymerization polymeric dispersant for replacing CMC in lithium battery as claimed in claim 1, wherein: the method comprises the steps of A, material preparation, B, heating and dissolving, C, synthesis reaction, D, cooling and E, packaging and discharging.
3. The preparation process of the emulsion polymerization polymeric dispersant for replacing CMC in lithium battery as claimed in claim 2, wherein: in the above-mentioned manner,
A. preparing materials: automatically weighing and feeding liquid raw materials, and manually feeding solid raw materials;
the method comprises three parts: firstly, pumping monomer vinyl acetate, butyl acrylate, isooctyl acrylate and other monomer materials into a pre-emulsification kettle, starting stirring for pre-emulsification to obtain pre-emulsion, secondly, adding an initiator and process water into the initiator kettle, uniformly stirring, thirdly, adding an emulsifier, process water and the like into a polymerization kettle, and uniformly stirring.
4. The preparation process of the emulsion polymerization polymeric dispersant for replacing CMC in lithium battery as claimed in claim 2, wherein: in the above-mentioned manner,
B. heating for dissolving: heating the polymerization kettle to 80-86 ℃, preserving heat for 10-30 minutes, and stirring and mixing uniformly.
5. The preparation process of the emulsion polymerization polymeric dispersant for replacing CMC in lithium battery as claimed in claim 2, wherein: in the above-mentioned manner,
C. and (3) synthesis reaction: dropwise adding a small amount of pre-emulsion into a polymerization kettle from a pre-emulsion kettle, continuously heating, adding a priming initiator when the temperature is raised to 78-84 ℃, and carrying out a priming reaction; after the bottoming reaction is finished, the pre-emulsion is dripped to carry out synthetic reaction, the temperature is controlled to be 80-86 ℃, the time is about 4-6 hours, and cooling water is added into a jacket of a reaction kettle to control the reaction temperature to be 80-86 ℃ along with the reaction.
6. The preparation process of the emulsion polymerization polymeric dispersant for replacing CMC in lithium battery as claimed in claim 2, wherein: in the above-mentioned manner,
D. and (3) cooling: after the polymerization reaction is finished, the temperature in the kettle is reduced to below 50 ℃ through the heat preservation process and the cooling, and the post-treatment agent is added for adjustment.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525399A (en) * | 2009-03-27 | 2009-09-09 | 上海应用技术学院 | Polyacrylate emulsion with high water resistance and preparation method thereof |
| CN113527572A (en) * | 2020-11-13 | 2021-10-22 | 深圳市研一新材料有限责任公司 | Aqueous thickening dispersant and aqueous binder for lithium ion battery and preparation method of aqueous thickening dispersant and aqueous binder |
| CN113613768A (en) * | 2019-03-29 | 2021-11-05 | 东洋油墨Sc控股株式会社 | Dispersant, dispersion, resin composition, composite material slurry, electrode film, and nonaqueous electrolyte secondary battery |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525399A (en) * | 2009-03-27 | 2009-09-09 | 上海应用技术学院 | Polyacrylate emulsion with high water resistance and preparation method thereof |
| CN113613768A (en) * | 2019-03-29 | 2021-11-05 | 东洋油墨Sc控股株式会社 | Dispersant, dispersion, resin composition, composite material slurry, electrode film, and nonaqueous electrolyte secondary battery |
| CN113527572A (en) * | 2020-11-13 | 2021-10-22 | 深圳市研一新材料有限责任公司 | Aqueous thickening dispersant and aqueous binder for lithium ion battery and preparation method of aqueous thickening dispersant and aqueous binder |
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