JPH0116855B2 - - Google Patents
Info
- Publication number
- JPH0116855B2 JPH0116855B2 JP60045668A JP4566885A JPH0116855B2 JP H0116855 B2 JPH0116855 B2 JP H0116855B2 JP 60045668 A JP60045668 A JP 60045668A JP 4566885 A JP4566885 A JP 4566885A JP H0116855 B2 JPH0116855 B2 JP H0116855B2
- Authority
- JP
- Japan
- Prior art keywords
- copolymer
- coating
- latex
- composition
- particle size
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 239000000203 mixture Substances 0.000 claims description 33
- 238000000576 coating method Methods 0.000 claims description 32
- 239000011248 coating agent Substances 0.000 claims description 30
- 229920001577 copolymer Polymers 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 22
- 239000006185 dispersion Substances 0.000 claims description 17
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 8
- 239000002736 nonionic surfactant Substances 0.000 claims description 7
- 239000003945 anionic surfactant Substances 0.000 claims description 5
- JMGNVALALWCTLC-UHFFFAOYSA-N 1-fluoro-2-(2-fluoroethenoxy)ethene Chemical compound FC=COC=CF JMGNVALALWCTLC-UHFFFAOYSA-N 0.000 claims description 4
- 125000000129 anionic group Chemical group 0.000 claims description 3
- 229920006026 co-polymeric resin Polymers 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- 239000010408 film Substances 0.000 description 27
- 239000004816 latex Substances 0.000 description 24
- 229920000126 latex Polymers 0.000 description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 238000006243 chemical reaction Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 238000006116 polymerization reaction Methods 0.000 description 13
- 230000003746 surface roughness Effects 0.000 description 11
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 7
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- BOSAWIQFTJIYIS-UHFFFAOYSA-N 1,1,1-trichloro-2,2,2-trifluoroethane Chemical compound FC(F)(F)C(Cl)(Cl)Cl BOSAWIQFTJIYIS-UHFFFAOYSA-N 0.000 description 5
- -1 polytetrafluoroethylene Polymers 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- YOALFLHFSFEMLP-UHFFFAOYSA-N azane;2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-pentadecafluorooctanoic acid Chemical compound [NH4+].[O-]C(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YOALFLHFSFEMLP-UHFFFAOYSA-N 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- 239000003381 stabilizer Substances 0.000 description 4
- OVGRCEFMXPHEBL-UHFFFAOYSA-N 1-ethenoxypropane Chemical compound CCCOC=C OVGRCEFMXPHEBL-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 239000012986 chain transfer agent Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 2
- 235000011613 Pinus brutia Nutrition 0.000 description 2
- 241000018646 Pinus brutia Species 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000012044 organic layer Substances 0.000 description 2
- 238000010422 painting Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 235000010893 Bischofia javanica Nutrition 0.000 description 1
- 240000005220 Bischofia javanica Species 0.000 description 1
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 1
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000047703 Nonion Species 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 1
- 150000001350 alkyl halides Chemical class 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- 229960001701 chloroform Drugs 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 description 1
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000009503 electrostatic coating Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- LRMHFDNWKCSEQU-UHFFFAOYSA-N ethoxyethane;phenol Chemical compound CCOCC.OC1=CC=CC=C1 LRMHFDNWKCSEQU-UHFFFAOYSA-N 0.000 description 1
- 229960003750 ethyl chloride Drugs 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical compound FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000007603 infrared drying Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010128 melt processing Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000007591 painting process Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000007592 spray painting technique Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Description
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The present invention relates to an aqueous dispersion composition, and more particularly to an aqueous dispersion composition of a tetrafluoroethylene/fluorovinyl ether copolymer, particularly a composition suitable for imparting non-stick properties by coating a substrate. relating to things. It is known to coat the surfaces of metals, ceramics, heat-resistant rubber, etc. with fluorocarbon polymers for various applications, such as polytetrafluoroethylene (PTFE) and tetrafluoroethylene/hexafluoropropene. Copolymers (FEP), tetrafluoroethylene/perfluoroalkyl vinyl ether copolymers (PFA), etc. are used to take advantage of their properties such as non-adhesiveness, heat resistance, chemical resistance, and low coefficient of friction. There is. PTFE-FEP is commercially available as an aqueous dispersion composition and is applied as a coating by spraying or dipping. Furthermore, FEP and PFA are used in electrostatic powder coating and are commercially available as powders of 5 to 150 ÎŒm. Examples of electrostatic powder coating include coatings on rolls of copying machines, as seen in, for example, JP-A-55-31494 and JP-A-58-24174. On the other hand, PTFE, FEP, and PFA can all be prepared as an aqueous dispersion, and examples are known in which an aqueous dispersion of FEP or PFA is mixed with an aqueous PTFE dispersion and used for coating. (For example, see Japanese Patent Publication No. 52-21531 and US Pat. No. 4,252,859).
However, there are almost no known examples of using PFA aqueous dispersions alone for coating purposes. For example, PFA aqueous dispersion is
It is prepared by the method described in No. The aqueous dispersion prepared according to the method of this patent is usually subjected to melt processing after separating the polymer and forming it into pellets or powder.
As shown in Figure 2, when this is applied to an aqueous dispersion composition, it can be applied only to an extremely thin film thickness, and if it is applied thickly, so-called mud cracks occur. Moreover, the surface of the coating film is also rough. The present invention aims to improve the drawbacks of such PFA aqueous dispersions, and the gist thereof is the general formula: (In the formula, X is H or F, n is a number from 0 to 7, m
is a number from 0 to 3. ) A copolymer of fluorovinyl ether and tetrafluoroethylene represented by particle size
An aqueous copolymer resin dispersion composition containing colloidal copolymer particles of 0.3 to 1 ÎŒm as a main component and stabilized with an anionic or nonionic surfactant. The composition of the present invention is composed of a colloidal tetrafluoroethylene/fluorovinyl ether copolymer aqueous dispersion, and can be coated in thick coats.
A smooth coating surface can be obtained. It is especially suitable for non-adhesive processing. Examples include fixing rolls for copying machines, food processing rolls, trays, and seasoning utensils. The colloidal copolymer particles, which are a requirement of the present invention, have an average particle diameter of 0.3 to 1 ÎŒm and a specific melt viscosity (MV) of 0.3 to 5Ã10 4 poise. Only with these characteristics can the objectives of the invention be achieved. The composition of the present invention is characterized by thick coating processability and smoothness of the coating film, but the copolymer particles of the present invention are also unprecedentedly large for PFA, which is why they have a specific MV. Therefore, better thick coating processability and coating film smoothness are achieved. When coating with the composition of the present invention, a coating film with a thickness of at least 25 ÎŒm or more (usually 35 ÎŒm or more) can be formed in one coating. Also, the surface roughness is 0.5ÎŒm
Small as below. Usually, commercially available PTFE or
The reality is that an aqueous dispersion composition of FEP can only provide a coating film with a thickness of about 10 to 20 ÎŒm. With such a film thickness, for example, when processing a fuser roll for a copying machine, it is necessary to apply the coating to a thickness that is the sum of the required film thickness and the amount of surface polishing after painting, but usually 25 ÎŒm.
The above-mentioned film thickness is insufficient for the required film thickness. On the other hand, electrostatic coating using FEP or PFA powder produces coatings with a thickness exceeding 100 ÎŒm. but,
On the contrary, this is too thick, resulting in a large amount of cutting (resulting in loss of raw materials), which is uneconomical and requires a large number of man-hours. When the surface roughness of the coating film formed by the composition of the present invention is small, it is often possible to put it into practical use without surface polishing. As a result of a detailed study of both particle size and MV physical properties, the inventor found that MV was 0.3 to 5.
Ã10 4 poise (preferably 0.4 to 3 Ã 10 4 poise),
It has been found that an average particle diameter of 0.3 to 1 ÎŒm (preferably 0.5 to 0.8 ÎŒm) is most suitable for the above purpose, and the present invention has been completed. Regarding MV, if it is too high than the above range, the surface roughness will be large even if the particle size is large, and pine cracks will be likely to occur. In this case as well, we ended up having to remove a lot,
Uneconomical problems become a problem, and even the required film thickness cannot be obtained. Of course, if it is too low than the above range, the mechanical strength will be low and it will become brittle. Since the colloidally dispersed particles of the present invention are much larger than those commonly known, it is necessary to increase the viscosity of the composition to make it less likely to settle. Furthermore, it must have the property of being easy to redisperse even if it settles once. Therefore, anionic or nonionic surfactants or mixtures thereof are added to the composition. Types of nonionic surfactants typically include reactions between ethylene oxide as a hydrophilic part and compounds such as propylene oxide, saturated and unsaturated aliphatic alcohols, and alkyl phenols as hydrophobic parts. It is a product. For example, oxyethylene, oxypropylene block copolymer, HO(C 2 H 4 O) a-
(C 3 H 6 O)b-(C 2 H 4 O)c H (molecular weight 1000~
4000, 18âŠa+b+câŠ85),
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ãŠãããã®ã§çŽ20ÎŒmã®èåã®ãã®ã§æ¯èŒããã[Formula] (d=4 to 20) is suitable. As the anionic surfactant, dialkyl sulfosuccinate, dodecylbenzenesulfonate, fatty acid soap, etc. can be used. In addition, water-soluble polymers or inorganic salts such as sodium alginate, polyvinyl alcohol, polyacrylates, and methylcellulose may be added to increase the viscosity of the composition. In addition, in order to further improve film-forming properties, water-insoluble organic solvents,
For example, it is also possible to disperse and emulsify benzene, toluene, xylene, etc. The nonionic or anionic surfactant used as a stabilizer is
20% by weight, preferably 4-10% by weight is suitable. If there is too much stabilizer, it will be difficult to volatilize during sintering and the coating performance will deteriorate. Furthermore, too much stabilizer and excessive thickener will make the painting process itself difficult. usually,
The viscosity of the composition of the present invention is 50 to 1000 at 25°C.
It is preferably adjusted to centipoise, preferably 100 to 400 centipoise. The content of the copolymer resin in the composition is preferably 20 to 65% based on the total weight of the composition. The composition of the present invention is first prepared by combining tetrafluoroethylene in an aqueous medium. (In the formula, n and m have the same meanings as above.) to perform emulsion polymerization, and then the obtained latex is concentrated, stabilized by adding a specified surfactant, and in some cases, further It can be manufactured by adding a thickener. In the emulsion copolymerization of the present invention, a so-called seed polymerization method is employed, and is characterized in that the final particle size is controlled by changing the amount of seeds. Furthermore, MV can be controlled by the amount of chain transfer agent, amount of initiator, reaction temperature, etc. As chain transfer agents, organic compounds containing hydrogen and present in substantially liquid form under the reaction conditions (e.g. methanol and ethanol) and alkyl halides (e.g. dichloromethane, trichloromethane, tetrachloroethane and chloroethane) may be used. . Examples of suitable polymerization initiators include water-soluble organic or inorganic peroxides such as disuccinic peroxide, ammonium persulfate, potassium persulfate, and the like. Additionally, reducing compounds such as ammonium sulfite, sodium bisulfite, sodium thiosulfate, etc. can also be used with the peroxides. Hereinafter, specific embodiments of the present invention will be illustrated by way of Examples. Example 1 First, a seed latex to be used for seed polymerization is synthesized by the method (1) (separately, a coating evaluation of the composition is carried out as Comparative Example 1). Thereafter, seed polymerization is performed by method (2). (1) In a stainless steel autoclave with an internal volume of 6 equipped with a temperature control jacket and a stirrer with anchor blades, add 2.9 g of deionized water, 400 g of trichlorotrifluoroethane as a dispersion stabilizer, 9.0 g of ammonium perfluorooctanoate, and chain transfer. Charge 2 ml of reagent grade methanol as a reagent, replace the inside of the tank for deoxidation twice with nitrogen gas and twice with TFE gas, and then charge 70 g of perfluor (propyl vinyl ether) (PPVE).
The temperature was raised to 65°C while stirring, and TFE gas was injected into the tank until the pressure within the tank reached 9.2 Kgf/cm 2 .
Then, 100 ml of an aqueous solution containing 4.2 g of ammonium persulfate (APS) is added to start the reaction. During the reaction, keep the pressure inside the tank at 9.2Kgf/ cm2 .
Continuously supply TFE gas, reaction temperature is 65±1â
is maintained. After 4.7 hours, the stirring is stopped, the autoclave is cooled to room temperature, and the gas is released back to atmospheric pressure. The copolymer concentration in the obtained latex is
The average particle diameter of the copolymer was 0.18 ÎŒm, the PPVE content in the copolymer was 3.2% by weight, and the MV of the copolymer was 1.0Ã10 4 poise. (2) After charging the same amount of deionized water, trichlorotrifluoroethane, and ammonium perfluorooctanoate into the same autoclave as in (1), add reagent special grade methanol in the amount listed in Table 1 (11 ml),
The amount of Terrax synthesized in (1) in Table 1 (250
g) After preparation and deoxidation, add 70g of PPVE. Thereafter, 4.2g of APS is added and the reaction is carried out in exactly the same manner as in (1). The reaction temperature and reaction pressure are also the same. The reaction time, latex properties, etc. are as shown in Table 1. Next, after the reaction of the raw latex obtained in (2) is completed, the organic phase (trichlorotrifluoroethane and unreacted PPVE) is separated and transferred to a separate container, and polyoxyethylene octyl phenol ether (NOF) Add a nonionic surfactant aqueous solution containing 20% by weight of Nonion HS-208) to each raw latex.
Mix 30g. Keep the mixture at 30±1°C and let it stand. After standing still for about 20 hours, the supernatant layer of the mixture separated into a concentrated latex layer and a supernatant layer is removed to obtain a latex with a copolymer concentration of 60% or more. To further stabilize this concentrated latex, water and nonionic
Add HS208 and adjust the copolymer concentration to 50% by weight and nonionic surfactant to 5% by weight (based on polymer weight). The prepared composition is subjected to coating and coating evaluation as described below. A portion of the latex immediately after polymerization is evaporated to dryness, washed with acetone, and dried to powder. The MV was measured with this powder and also at 350â.
Heat press for 15 minutes to create a film with a thickness of approximately 0.05 mm, and quantify the perfluor (propyl vinyl ether) content in the copolymer using infrared spectroscopy. The crack limit thickness of this example was 26 to 30 ÎŒm, and the surface roughness was 0.40 ÎŒm. On the other hand, in Comparative Example 1, the critical thickness was small and the surface roughness was rough (large). The effect of particle size is significant. Examples 2-5 In Example 2, the same seed latex used in Example 1 was used to carry out the seed polymerization. Example 3~
In Example 5, seed polymerization was carried out using part of the raw latex obtained in Example 1 as a seed (therefore, as a result, seed polymerization was carried out twice). The amounts of methanol and ammonium persulfate used are as listed in Table 1, and all conditions other than those listed in Table 1 are the same as in Example 1. As shown in Table 2, all had excellent coating film properties. Example 6 In the method of step (1) of Example 1, deionized water, trichlorotrifluoroethane, ammonium perfluorooctanoate, and PPVE were used in the same amounts, and as a chain transfer agent, reagent special grade was used instead of methanol. 66g of dichloromethane was used. The polymerization temperature was 35° C., and the reaction was started by adding 50 ml of an aqueous solution containing 4.2 g of ammonium persulfate, followed by the addition of 50 ml of an aqueous solution containing 2.3 g of sodium sulfite.
During the reaction, tetrafluoroethylene was supplied so as to keep the internal pressure at 9.2 Kgf/cm 2 and the polymerization temperature was maintained at 35±1°C. After 9.6 hours, the reaction was terminated in the same manner as in step (1) of Example 1, and a latex with a polymer concentration of 19.0% by weight and an average particle size of 0.18 ÎŒm was obtained, and the MV of the copolymer was 3.3Ã10 4 poise. , the PPVE content was 2.7%. Furthermore, using 250 g of this latex as a seed, the same amount of deionized water as above, trichlorotrifluoroethane, ammonium perfluorooctanoate,
The mixture was charged into an autoclave with PPVE, and then 90 g of dichloromethane was added as a chain transfer agent, and the same amounts of ammonium persulfate and sodium sulfite as above were added to carry out seed polymerization. reaction pressure,
The reaction temperature was the same as for the synthesis of the seed latex. After 14 hours, the latex had a polymer concentration of 18.7% and an average particle size of 0.35 ÎŒm. The MV of the copolymer was 2.1Ã10 4 poise, and the PPVE content was 3.0% by weight. The raw latex thus obtained was subjected to organic layer separation, concentration, stabilization, and adjustment in the same manner as in Example 1, and the coating and coating film were evaluated. The crack thickness limit was 30 to 35 ÎŒm, and the surface roughness was 0.50 ÎŒm. Comparative Examples 1 to 5 Comparative Example 1 is the seed latex composition of Example 1, and Comparative Examples 2 to 3 are seed latex compounds without seed polymerization.
This is a method for producing seed latex in Example 1 in which the amount of methanol was changed to change the MV. Comparative Example 4 used the raw latex of Comparative Example 2, and Comparative Example 5 used the raw latex of Comparative Example 1, and seed polymerization was carried out under the conditions shown in Table 1 according to Example 1. The physical properties of the coating film are as shown in Table 2, and Comparative Example 4
Even if the particle size is large, the MV is too high and the surface roughness is large. Comparative Example 5 has good crack limit film thickness and surface roughness, but in this case,
This is probably because the MV is too small, but the coating film strength is low and it is almost impractical. Comparative Example 6 Seed latex used in Example 6 (average particle size
0.18 ÎŒm, MV 3.3Ã10 4 poise, PPVE content 2.7% by weight) was separated, concentrated, stabilized, and adjusted in the same manner as in Example 1, and then painted and evaluated. The crack limit thickness is 20~25ÎŒm, and the surface roughness is
It was 0.80 Όm. In addition, in Examples 2 to 6 and Comparative Examples 1 to 5, the organic layer separation, concentration, stabilization, and adjustment were performed as described in Example 1, and the coating and coating film evaluation were performed under the same conditions. <Specific melt viscosity> Using a Koka type flow tester made by Shimadzu Corporation, 2.0 g of copolymer powder was loaded into a cylinder with an inner diameter of 11.3 mm, and after keeping at a temperature of 380°C for 5 minutes, the inner diameter was 2.1 mm under a piston load of 7 kg. mm, extrusion through an orifice with a length of 8 mm, extrusion speed (g/min)
The specific melt viscosity (poise) was determined by dividing 53150 by . <Average particle size> Regarding the latex immediately after the completion of polymerization of the concentrate,
Photographs were taken with a transmission electron microscope, and the directional length and diameter of about 100 to 400 particles were measured to determine the average length diameter. <Fluorovinyl ether content in the copolymer> Regarding perfluorinated (propyl vinyl ether) in the copolymer, the above-mentioned film was measured by infrared spectroscopy to determine the absorbance at 995 cm -1 relative to the absorbance at 2360 cm -1 .
It was determined by multiplying the absorbance ratio by 0.95 (see JP-A-56-92943). <Painting test> The prepared aqueous dispersion composition was coated with a width of 5 cm and a length of 40 cm.
Spray painting on a 1 mm thick aluminum plate (previously cleaned with acetone and deoiled). Spray gun nozzle diameter is 0.8~1.1
mm, and the air pressure is approximately 3Kg/cm 2 . At this time, the amount of the composition sprayed on each part of the aluminum plate is changed appropriately so that the thickness after firing is 10 to 50 ÎŒm. After spraying, infrared drying oven (approx. 100â)
Pre-dry for 10 minutes, then place in an electric furnace controlled at 400°C and bake for 20 minutes. Immediately after firing, remove from the furnace and allow to cool to room temperature. <Evaluation of paint film> Measure the thickness of the paint film using a surface film thickness meter. As the film thickness increases, mound cracks are observed, but the maximum film thickness without mound cracks is defined as the crack limit thickness. Universal surface profile measuring device for surface roughness (Kosaka Institute Co., Ltd.)
Measured using SE-3C). Since the surface roughness varies depending on the film thickness, we will compare the film thickness of approximately 20 ÎŒm.
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[Table] ** The resulting paint film developed pine cracks after a few days.
Claims (1)
ïœã¯ïŒãïŒã®æŽæ°ã§ãããïŒ ã§è¡šãããããã«ãªã«ããã«ãšãŒãã«ãšããã©ã
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èç²åºŠã0.3Ã104ãïŒÃ104ãã€ãºãå¹³åç²åŸã
0.3ã1ÎŒmã®ã³ãã€ãç¶å ±éåäœç²åãäž»æåãš
ããŠå«ã¿ãã¢ããªã³æ§ãŸãã¯ãããªã³æ§çé¢æŽ»æ§
å€ã§å®å®åãããå ±éåäœæš¹èæ°Žæ§åæ£æ¶²çµæ
ç©ã ïŒ ãã«ãªã«ããã«ãšãŒãã«ãC3F7OCFïŒCF2ã§
ããç¹èš±è«æ±ã®ç¯å²ç¬¬ïŒé èšèŒã®çµæç©ã ïŒ å¹³åç²åŸã0.5ÎŒmãã倧ãããæ¯æº¶èç²åºŠã
0.4ã3.0Ã104ãã€ãºã§ããç¹èš±è«æ±ã®ç¯å²ç¬¬ïŒé
èšèŒã®çµæç©ã ïŒ å¹³åç²åŸã0.6ã0.8ÎŒmã§ããç¹èš±è«æ±ã®ç¯å²
第ïŒé èšèŒã®çµæç©ã ïŒ éç²çå¡è£ çšã®ç¹èš±è«æ±ã®ç¯å²ç¬¬ïŒé èšèŒã®
çµæç©ã[Claims] 1. General formula: (In the formula, X is H or F, n is an integer of 0 to 7,
m is an integer from 0 to 3. ) A copolymer of fluorovinyl ether and tetrafluoroethylene represented by particle size
An aqueous copolymer resin dispersion composition containing colloidal copolymer particles of 0.3 to 1 ÎŒm as a main component and stabilized with an anionic or nonionic surfactant. 2. The composition according to claim 1, wherein the fluorovinyl ether is C3F7OCF = CF2 . 3 The average particle size is larger than 0.5 ÎŒm and the specific melt viscosity is
The composition according to claim 1, which has a poise of 0.4 to 3.0Ã10 4 poise. 4. The composition according to claim 1, having an average particle size of 0.6 to 0.8 ÎŒm. 5. The composition according to claim 1 for non-adhesive coating.
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP4566885A JPS61204253A (en) | 1985-03-06 | 1985-03-06 | Aqueous dispersion composition |
DE8686103004T DE3682086D1 (en) | 1985-03-06 | 1986-03-06 | AQUEOUS DISPERSION OF A FLUORINE COPOLYMER AND ITEM COATED WITH IT. |
EP19860103004 EP0193963B1 (en) | 1985-03-06 | 1986-03-06 | Aqueous dispersion comprising fluorine-containing copolymer and article coated therewith |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP4566885A JPS61204253A (en) | 1985-03-06 | 1985-03-06 | Aqueous dispersion composition |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS61204253A JPS61204253A (en) | 1986-09-10 |
JPH0116855B2 true JPH0116855B2 (en) | 1989-03-28 |
Family
ID=12725763
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP4566885A Granted JPS61204253A (en) | 1985-03-06 | 1985-03-06 | Aqueous dispersion composition |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS61204253A (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2023224050A1 (en) * | 2022-05-19 | 2023-11-23 | ïœïœæ ªåŒäŒç€Ÿ | Method for producing aqueous dispersion, and aqueous dispersion |
-
1985
- 1985-03-06 JP JP4566885A patent/JPS61204253A/en active Granted
Also Published As
Publication number | Publication date |
---|---|
JPS61204253A (en) | 1986-09-10 |
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