CN115926195A - Preparation method and application of polyolefin microsphere emulsion with low dispersant content - Google Patents
Preparation method and application of polyolefin microsphere emulsion with low dispersant content Download PDFInfo
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Abstract
The invention provides a polyolefin microsphere with low dispersant content, a preparation method and application thereof, belonging to the technical field of polyolefin microsphere preparation. The method comprises the steps of carrying out surface oxidation on polyolefin powder, then dispersing in water, adding an emulsifier to form an emulsion, then dropwise adding an acrylate monomer under the protection of nitrogen to carry out free radical emulsion polymerization to obtain polyolefin microsphere emulsion, carrying out spray drying on the polyolefin microsphere emulsion to obtain polyolefin microsphere powder, and adding a dispersing agent into the polyolefin microsphere powder to obtain the polyolefin microsphere emulsion with low dispersing agent content. The invention also provides application of the polyolefin microsphere emulsion in preparation of a coated diaphragm. The invention uses less than 0.5 percent of dispersant in the preparation process, the content of the dispersant is low, and simultaneously, the surface of the polyolefin is provided with the acrylate which has certain adhesive capacity, thereby avoiding the problems of hole blocking and internal resistance increase of the battery caused by a large amount of emulsifier.
Description
Technical Field
The invention belongs to the technical field of preparation of polyolefin microsphere emulsion, and particularly relates to a preparation method and application of polyolefin microsphere emulsion with low dispersant content.
Background
The polyolefin material is a high polymer material with easily obtained raw materials and stable performance, and can be used as a coating raw material of a diaphragm in the field of lithium batteries. However, because polyolefin has weak polarity and strong hydrophobicity, more than 10wt% of dispersing agent needs to be added in the preparation process when the polyolefin is prepared into microsphere emulsion for use. The addition of a large amount of dispersant can cause the blocking of pores of the diaphragm, which leads to the increase of the ventilation of the diaphragm, thereby causing the increase of the internal resistance of the battery and the influence of the stability of the lithium battery.
Disclosure of Invention
The invention discloses a preparation method and application of polyolefin microsphere emulsion with low dispersant content.
The invention firstly provides a preparation method of polyolefin microsphere emulsion with low dispersant content, which comprises the following steps:
the method comprises the following steps of carrying out surface oxidation on polyolefin powder, then dispersing in water, adding an emulsifier to form an emulsion, dropwise adding an acrylate monomer under the protection of nitrogen to carry out free radical emulsion polymerization to obtain polyolefin microsphere emulsion, carrying out spray drying on the polyolefin microsphere emulsion to obtain polyolefin microsphere powder, and adding a dispersant into the polyolefin microsphere powder to obtain the polyolefin microsphere emulsion with low dispersant content.
Preferably, the polyolefin powder comprises polyethylene, polypropylene, polybutylene homo-or copolymer powder.
Preferably, the content of the dispersant is less than 0.5%.
Preferably, the dispersant is one or both of an anionic dispersant and a nonionic dispersant.
Preferably, the anionic dispersant is alkyl sulfate, alkyl benzene sulfonate, phosphate; the nonionic dispersing agent is polyoxyethylene ether, polyoxypropylene ether, segmented copolymer of ethylene oxide and propylene oxide, polyol fatty acid ester or polyvinyl alcohol.
Preferably, the acrylate comprises one or more of acrylate, methacrylate, ethyl acrylate or cyanoacrylate.
Preferably, the mass ratio of the polyolefin powder to the acrylic monomer is 1: (0.001-0.01).
Preferably, the temperature of the spray drying is 100-300 ℃ and the time is 2-60s.
The invention also provides the polyolefin microsphere emulsion with low dispersant content obtained by the preparation method.
The invention also provides application of the polyolefin microsphere emulsion with low dispersant content in preparation of a coating membrane.
The invention has the advantages of
The invention discloses a preparation method and application of polyolefin microsphere emulsion with low dispersant content, wherein polyolefin microsphere particles are of a core-shell structure consisting of a polyolefin core and an acrylate shell, and the particle size of the polyolefin microspheres is less than 2um; in the preparation process of the microsphere emulsion, the surface polarity is increased through the surface oxidation treatment of polyolefin powder, and the acrylic ester polar monomer is grafted, so that the surface hydrophilicity is greatly increased, and the content of the dispersing agent of the polymer microsphere during the stabilization in water is reduced. The prepared polyolefin microsphere coating diaphragm has good bonding strength with the positive and negative pole pieces, and simultaneously avoids the problems of hole blockage, black spot lithium precipitation, increased internal resistance of the battery and insufficient cycle life caused by a large amount of dispersing agents.
Compared with the prior art, the invention uses less than 0.5 percent of dispersant in the preparation process, the content of the dispersant is low, meanwhile, the surface of the microsphere is provided with the acrylate, the microsphere has certain bonding capability, the dosage of the adhesive, the dispersant and the wetting agent in coating is greatly reduced, the material cost is saved, and the problems of hole blocking, internal resistance increase of a battery and the like caused by the adhesive dispersant are also avoided.
Detailed Description
The invention firstly provides a preparation method of polyolefin microsphere emulsion with low dispersant content, which comprises the following steps:
the method comprises the steps of carrying out surface oxidation on polyolefin powder, then dispersing in water, adding an emulsifier to form an emulsion, then dropwise adding an acrylate monomer under the protection of nitrogen to carry out free radical emulsion polymerization to obtain polyolefin microsphere emulsion, carrying out spray drying on the polyolefin microsphere emulsion to obtain polyolefin microsphere powder, and adding a dispersing agent into the polyolefin microsphere powder to obtain the polyolefin microsphere emulsion with low dispersing agent content.
According to the invention, the polyolefin powder is first subjected to surface oxidation by means well known in the art, preferably by means of corona or irradiation, preferably by: the polyolefin powder is at 8000-9000V/m 2 The surface oxidation treatment is carried out under the action of high-frequency high-voltage electricity, the surface polarity is increased by the surface oxidation treatment of the polyolefin powder, and the polar monomer of acrylic ester is grafted, so that the surface hydrophilicity is greatly increased, the content of the dispersing agent when the polymer microspheres are stable in water is reduced, stable and dispersed emulsion can be formed by only adding a small amount of the dispersing agent and water, and the content of the dispersing agent is reduced.
According to the invention, the polyolefin powders are commercially available, preferably comprising polyethylene, polypropylene, polybutylene homo-or copolymer powders.
According to the invention, the content of emulsifier is less than 0.5%, preferably 0.2% to 0.4%. The emulsifier is preferably one or both of an anionic emulsifier and a nonionic emulsifier.
The anionic emulsifier is preferably alkyl sulfate, alkylbenzene sulfonate or phosphate; more preferably sodium dodecylbenzene sulfonate; the nonionic emulsifier is preferably polyoxyethylene ether, polyoxypropylene ether, block copolymer of ethylene oxide and propylene oxide, polyol fatty acid ester or polyvinyl alcohol, more preferably polyoxyethylene ether.
According to the invention, the acrylate monomer preferably comprises one or more of acrylate, methacrylate, ethyl acrylate or cyanoacrylate. According to the invention, the acrylate monomer is dripped on the surface of the polyolefin, the polyolefin microspheres with core-shell structures are formed through free radical emulsion polymerization, and the acrylate monomer has certain bonding capacity, so that the prepared polyolefin microsphere diaphragm has good bonding strength with positive and negative pole pieces, and simultaneously, the use amounts of a large amount of emulsifier, adhesive, dispersant and wetting agent are avoided, and the problems of hole blockage and increased internal resistance of the battery are avoided.
According to the invention, the mass ratio of the polyolefin powder to the acrylic monomer is preferably 1:
(0.001-0.01), more preferably 1: (0.0015-0.0023).
According to the invention, the polymerization temperature is preferably from 75 to 90 ℃ and more preferably from 82 to 85 ℃ and the time is preferably from 20 to 30 min and more preferably from 20 to 25 min.
According to the invention, the content of said dispersant is less than 0.5%, preferably between 0.2% and 0.4%. The dispersant is preferably one or both of an anionic dispersant and a nonionic dispersant.
The anionic dispersant is preferably alkyl sulfate, alkylbenzene sulfonate or phosphate; more preferably sodium dodecylbenzene sulfonate; the nonionic dispersant is preferably polyoxyethylene ether, polyoxypropylene ether, a block copolymer of ethylene oxide and propylene oxide, a polyol fatty acid ester or polyvinyl alcohol, and more preferably polyoxyethylene ether.
According to the invention, the spray drying is to atomize the emulsion into small droplets in the air, the small droplets contact with hot air in a drying chamber, the moisture is instantly evaporated at high temperature, the droplets are dried into fine powder and fall into the bottom of the drying chamber, and the solid content of the emulsion is 10-40 percent; the spray-drying temperature is preferably from 100 to 300 ℃ and the time is preferably from 2 to 60s.
According to the invention, the dispersing temperature of the added dispersing agent is preferably 5-80 ℃, and the dispersing time is preferably 20-300 min.
The invention also provides the polyolefin microsphere emulsion with low dispersant content obtained by the preparation method. The polyolefin microsphere emulsion obtained by the preparation method has a core-shell structure consisting of a polyolefin core and an acrylate shell, and the particle size of the polyolefin microsphere is less than 2um.
The invention also provides application of the polyolefin microsphere emulsion with low dispersant content in preparation of a coating membrane.
The preparation method of the polyolefin microsphere emulsion coating membrane comprises the following steps:
the method comprises the following steps: pulping: adding the polyolefin microsphere emulsion into water, sequentially adding the adhesive and the wetting agent, and stirring to form uniform coating liquid;
step two: coating: coating the prepared coating liquid on one or both surfaces of a lithium/sodium battery/supercapacitor separator;
step three: and (3) drying: and drying the coated membrane to obtain the polyolefin microsphere coated membrane.
According to the invention, the adhesive and the wetting agent are not particularly limited, and are selected according to the conventional types in the field, the adhesive is preferably one or more of polyacrylic acids, polyacrylates, polyacrylonitrile and modified copolymers thereof, polypropylene and modified copolymers thereof, and polyurethanes, more preferably polyacrylic acid, the wetting agent is preferably one or more of polyethers, polyethylene oxides and modified copolymers thereof, and fluoropolymers, and more preferably polyether. The mass ratio of the polyolefin microsphere emulsion, the adhesive and the wetting agent is preferably (65-95): (0.1-20): (1-5).
The present invention is further illustrated by reference to the following specific examples, in which the starting materials are all commercially available.
Example 1
200g of polyethylene powder is mixed at 8000V/m 2 After surface oxidation treatment under the action of high-frequency high-voltage electricity, adding the mixture into 800g of water, adding 0.5g of polyoxyethylene ether serving as an emulsifier, dropwise adding 0.3g of methacrylate monomer under the protection of nitrogen, stirring at 82 ℃ for 20 min to carry out emulsion polymerization to obtain polyolefin microsphere emulsion with a core-shell structure, atomizing the emulsion into small droplets in the air, contacting with 150 ℃ hot air in a drying chamber for 2s, instantly evaporating water at high temperature, drying the droplets into fine powder, and allowing the fine powder to fall into the bottom of the drying chamber to obtain the polyolefin microsphere emulsionThe powder was added with 1g of polyoxyethylene ether and 500g of water and stirred at 25 ℃ for 30 min to form an emulsion.
50g of the emulsion, 80g of deionized water, 3g of polyacrylic acid and 4g of polyether wetting agent are prepared into uniform coating liquid together, the coating liquid is coated on one surface of a lithium battery diaphragm with the thickness of 16 microns, and the polyolefin microsphere coated diaphragm is obtained after drying. The test properties are shown in table 1.
Example 2
300g of polypropylene powder is added at 9000V/m 2 After surface oxidation treatment under the action of high-frequency high-voltage electricity, adding the mixture into 700g of water, adding 1g of sodium dodecyl benzene sulfonate as an emulsifier, dropwise adding 0.7g of cyanoacrylate monomer under the protection of nitrogen, and stirring 20 min at 85 ℃ to carry out emulsion polymerization to obtain the polyolefin microsphere emulsion with the core-shell structure. Atomizing the emulsion into small droplets in the air, contacting with 160 ℃ hot air in a drying chamber for 2s, instantly evaporating water at high temperature, drying the droplets into fine powder, dropping the fine powder into the bottom of the drying chamber to obtain polyolefin microsphere powder, adding 0.8g of phosphate and 1000g of water, and stirring at 25 ℃ for 30 min to form the emulsion.
60g of the emulsion, 80g of deionized water, 3g of polyacrylic acid and 4g of polyether wetting agent are prepared into uniform coating liquid together, the coating liquid is coated on one surface of a lithium battery diaphragm with the thickness of 16 microns, and the polyolefin microsphere coated diaphragm is obtained after drying. The test performance is shown in table 1.
Comparative example 1
Adding 20g of polyethylene powder into 80g of water, adding 2.2g of emulsifier polyoxyethylene ether, stirring 20 min for dispersion to obtain polyolefin microspheres, and obtaining dispersion liquid;
100g of the dispersion liquid, 50g of deionized water, 3g of polyacrylic acid and 4g of polyether wetting agent are prepared into uniform coating liquid, the coating liquid is coated on one surface of a lithium battery diaphragm with the thickness of 16 microns, and the polyolefin microsphere coated diaphragm is obtained after drying. The test performance is shown in table 1.
Comparative example 2
Adding 200g of polyethylene powder into 800g of water, adding 0.5g of polyoxyethylene ether serving as an emulsifier, dropwise adding 0.3g of methacrylate monomer under the protection of nitrogen, stirring at 82 ℃ for 20 min to carry out emulsion polymerization to obtain polyolefin microsphere emulsion with a core-shell structure, atomizing the emulsion into small droplets in the air, contacting with 150 ℃ hot air in a drying chamber for 2s, instantly evaporating water at high temperature, drying the droplets into fine powder, falling to the bottom of the drying chamber to obtain polyolefin microsphere powder, adding 1g of polyoxyethylene ether and 500g of water, and stirring at 25 ℃ for 30 min to form the emulsion.
50g of the emulsion, 80g of deionized water, 3g of polyacrylic acid and 4g of polyether wetting agent are prepared into uniform coating liquid together, the coating liquid is coated on one surface of a lithium battery diaphragm with the thickness of 16 microns, and the polyolefin microsphere coated diaphragm is obtained after drying. The test properties are shown in table 1.
Comparative example 3
200g of polyethylene powder is mixed at 8000V/m 2 After surface oxidation treatment under the action of high-frequency high-voltage electricity, adding the mixture into 800g of water, adding 0.5g of emulsifier polyoxyethylene ether, stirring for 20 min at 82 ℃ to obtain polyolefin microsphere emulsion, atomizing the emulsion into small droplets in the air, contacting with 150 ℃ hot air in a drying chamber for 2s, instantly evaporating water at high temperature, drying the droplets into fine powder, falling into the bottom of the drying chamber to obtain polyolefin microsphere powder, adding 1g of polyoxyethylene ether and 500g of water, and stirring for 30 min at 25 ℃ to form the emulsion.
50g of the emulsion, 80g of deionized water, 3g of polyacrylic acid and 4g of polyether wetting agent are prepared into uniform coating liquid together, the coating liquid is coated on one surface of a lithium battery diaphragm with the thickness of 16 microns, and the polyolefin microsphere coated diaphragm is obtained after drying. The test performance is shown in table 1.
TABLE 1
In addition, the 100 batteries prepared in the comparative example 1 have 16 water jumps of 400-700 weeks, and the capacity is lower than 70 percent after 8 batteries are circulated for 1500 times; 10 soft package batteries bulge, and 9 black spots appear after disassembly; the 100 batteries prepared in the comparative example 2 have 19 jumping water of 400-700 weeks, and the capacity is lower than 70 percent after 10 cycles for 1500 times; 7 soft package batteries bulge, and 4 black spots appear after disassembly; the 100 batteries prepared in the comparative example 3 have 43 water jumps of 400-700 weeks, and the capacity is lower than 50% after 12 cycles of 1500 times; 13 soft-package batteries bulge, and 13 black spots appear after disassembly; on the other hand, in the case of 100 batteries manufactured in the same manner as in examples 1 and 2 of the present invention, no water jump occurred, the capacity was not lower than 80% after 1500 cycles, and no defects such as black spots were observed after disassembling the batteries.
The results show that the separators in the examples 1 and 2 have lower air permeability value and lower internal resistance of the battery, have higher dry-wet adhesive strength with the pole piece, and still have more than 80% of capacity retention rate after 1500 cycles of the battery.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A preparation method of polyolefin microsphere emulsion with low dispersant content is characterized by comprising the following steps:
the method comprises the steps of carrying out surface oxidation on polyolefin powder, then dispersing in water, adding an emulsifier to form an emulsion, then dropwise adding an acrylate monomer under the protection of nitrogen to carry out free radical emulsion polymerization to obtain polyolefin microsphere emulsion, carrying out spray drying on the polyolefin microsphere emulsion to obtain polyolefin microsphere powder, and adding a dispersing agent into the polyolefin microsphere powder to obtain the polyolefin microsphere emulsion with low dispersing agent content.
2. The method of claim 1, wherein the polyolefin powder comprises polyethylene, polypropylene, polybutylene homo-or copolymer powder.
3. The method for preparing polyolefin microsphere emulsion with low dispersant content as claimed in claim 1, wherein the dispersant content is less than 0.5%.
4. The method for preparing polyolefin microsphere emulsion with low dispersant content according to claim 1, wherein the dispersant is one or both of anionic dispersant and nonionic dispersant.
5. The method for preparing polyolefin microsphere emulsion with low dispersant content according to claim 4, wherein the anionic dispersant is alkyl sulfate, alkyl benzene sulfonate, phosphate; the non-ionic dispersing agent is polyoxyethylene ether, polyoxypropylene ether, segmented copolymer of ethylene oxide and propylene oxide, polyol fatty acid ester or polyvinyl alcohol.
6. The method for preparing polyolefin microsphere emulsion with low dispersant content according to claim 1, wherein the acrylate comprises one or more of acrylate, methacrylate, ethyl acrylate or cyanoacrylate.
7. The method for preparing polyolefin microsphere emulsion with low dispersant content according to claim 1, wherein the mass ratio of the polyolefin powder to the acrylic monomer is 1: (0.001-0.01).
8. The method for preparing polyolefin microsphere emulsion with low dispersant content according to claim 1, wherein the temperature of spray drying is 100-300 ℃ and the time is 2-60s.
9. The method of claim 1 wherein the low dispersant content polyolefin microsphere emulsion is obtained.
10. Use of the low dispersant content polyolefin microsphere emulsion of claim 9 for the preparation of a coated separator.
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