WO2023106287A1 - Composition d'un agent de traitement pour élimination des poussières - Google Patents

Composition d'un agent de traitement pour élimination des poussières Download PDF

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WO2023106287A1
WO2023106287A1 PCT/JP2022/044902 JP2022044902W WO2023106287A1 WO 2023106287 A1 WO2023106287 A1 WO 2023106287A1 JP 2022044902 W JP2022044902 W JP 2022044902W WO 2023106287 A1 WO2023106287 A1 WO 2023106287A1
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dust
agent composition
aqueous dispersion
melt
mass
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PCT/JP2022/044902
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English (en)
Japanese (ja)
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厳 江頭
一雄 小鍋
正輝 麦沢
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三井・ケマーズ フロロプロダクツ株式会社
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F214/00—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 a halogen
    • C08F214/18—Monomers containing fluorine
    • C08F214/26—Tetrafluoroethene
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/22—Materials not provided for elsewhere for dust-laying or dust-absorbing

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  • the present invention relates to a dust-suppressing treatment agent composition that has excellent performance in suppressing dust from dust-generating substances and is also excellent in redispersibility.
  • Dust inhibition of a dust-generating substance comprising an aqueous dispersion of a copolymer, wherein the redispersion sedimentation rate of the TFE copolymer is 60% or less, and the content of perfluorooctanoic acid and its salts is less than 10 ppb It relates to a treatment composition.
  • Patent Document 1 PTFE (TFE polymer) is mixed with a powdery substance, and the mixture is subjected to a compression-shearing action at a temperature of about 20 to 200 ° C. to make TFE heavy. Methods have been proposed for suppressing dusting of powdery substances by fibrillating coalescence.
  • TFE polymer described in Patent Document 1 below is a homopolymer of TFE as a composition, Teflon (registered trademark) 6 or Teflon (registered trademark) 30 as a fine powder or emulsion as a composition, and TFE as a composition. It is a modified polymer of Teflon (registered trademark) 6C, which is a fine powder.
  • Patent Document 2 a dust suppression method using a stable aqueous emulsion containing 1.0% by mass or more of a hydrocarbon-based anionic surfactant with respect to a homopolymer of TFE (TFE polymer) is used. has been proposed and shown to have a dust-suppressing effect on powdery substances.
  • particles of the TFE polymer are prepared by the emulsion polymerization method disclosed in Patent Documents 3 and 4 below, that is, an anionic interface using TFE as a water-soluble polymerization initiator and a fluoroalkyl group as a hydrophobic group.
  • aqueous emulsion It is produced in the form of an aqueous emulsion by injecting an active agent (hereinafter referred to as a fluorine-containing emulsifier) into an aqueous medium containing an emulsifier and polymerizing it, and an emulsion stabilizer is added to increase the stability.
  • an active agent hereinafter referred to as a fluorine-containing emulsifier
  • Patent Document 5 discloses that the use of a dust-suppressing treatment agent composition comprising an aqueous dispersion of a fluoropolymer having a fluorine-containing emulsifier content of 50 ppm or less has a dust-suppressing effect and is environmentally friendly. A method is described that can suppress dust without worrying about its effects.
  • the TFE polymer aqueous dispersion used as the dust-suppressing treatment agent composition in these methods tends to settle when left standing for a long period of time, and once the TFE polymer settles, it solidifies and is difficult to redisperse. There is a problem. Furthermore, depending on the conditions of use, the TFE polymer may not be able to exhibit its original dust-suppressing effect, such as a decrease in the concentration of the TFE polymer in the TFE polymer aqueous dispersion.
  • the present invention has an excellent dust suppressing effect and is also effective in the redispersibility of the non-melt-flowable TFE copolymer particles, which are the solid content in the dust suppressing treatment agent composition after being left standing for a long period of time.
  • An object of the present invention is to provide a dust-suppressing treatment agent composition which is excellent in environmental performance.
  • the present invention comprises a non-melt-flowable TFE copolymer aqueous dispersion, the copolymer represented by the following formula (1) has a redispersion sedimentation rate of 60% or less, and the perfluoropolymer in the aqueous dispersion
  • a dust-suppressing treatment composition of a dust-generating substance characterized in that the content of octanoic acid and its salts is less than 10 ppb.
  • Redispersion sedimentation rate (%) X 3 /X 2 ⁇ 100 (1)
  • X 2 15 g of an aqueous dispersion of a TFE polymer having the same concentration as the copolymer was centrifuged at a temperature of 20°C and a rotation speed of 3000 rpm for 30 minutes using a centrifuge, and then re-dispersed.
  • X 3 15 g of the aqueous dispersion of the copolymer was heated to 20°C and rotated at a speed of 300.
  • Solid sedimentation ratio after redispersion (%) (Amount of sedimentation of solid content after redispersion) / (Amount of solid content before centrifugation) x 100 ...
  • the amount of perfluorooctanoic acid and its salt is less than 5 ppb relative to the mass of the aqueous dispersion.
  • the particle size (d84) is 250 nm or less when the cumulative volume percentage of the copolymer is 84%.
  • the non-melt-flowable TFE copolymer is a non-melt-flowable copolymer of TFE and at least one comonomer selected from (perfluoroalkyl)ethylene, perfluoro(alkyl vinyl ether), and hexafluoropropylene. Being polymeric is a preferred aspect of the present invention.
  • the perfluoroalkyl group in the (perfluoroalkyl)ethylene is a perfluoroalkyl group having 1 to 10 carbon atoms.
  • the (perfluoroalkyl)ethylene is at least one selected from (perfluoroethyl)ethylene, (perfluorobutyl)ethylene, (perfluorohexyl)ethylene, and (perfluorooctyl)ethylene. This is a preferred embodiment of the invention.
  • the perfluoroalkyl group in the perfluoro(alkyl vinyl ether) is a perfluoroalkyl group having 1 to 10 carbon atoms.
  • the perfluoro(alkyl vinyl ether) is at least one selected from perfluoro(methyl vinyl ether), perfluoro(ethyl vinyl ether), and perfluoro(propyl vinyl ether). .
  • the comonomer is contained in an amount of 0.01 to 1.00% by mass with respect to TFE.
  • the comonomer is contained in an amount of 0.01 to 0.50% by mass with respect to TFE.
  • the copolymer is contained in the dust control agent composition at a concentration of 10 to 80% by mass.
  • the specific gravity (SSG) of the copolymer is 2.27 or less.
  • the present invention also provides a dust suppressing treatment agent powder of a dust-generating substance, which is obtained by granulating and then drying the dust suppressing treatment agent composition.
  • the dust-generating substance is a dust-generating powdery substance.
  • non-melt-flowable TFE copolymer particles that are solids in the dust suppressing treatment agent composition even after standing for a long period of time
  • a dust-suppressing treatment agent composition of a dust-generating substance which is excellent in redispersibility of dust and environmental performance.
  • FIG. 1 is a diagram showing the results of centrifugal sedimentation tests and centrifugal sedimentation redispersion tests of Examples 1 to 3 and Comparative Example 1.
  • FIG. 1 is a diagram showing the results of static sedimentation tests and static sedimentation redispersion tests of Examples 1 and 2 and Comparative Example 1.
  • FIG. 2 is a photograph of Example 2 and Comparative Example 1 after standing for 90 days.
  • the dust-suppressing treatment composition of the dust-generating substance of the present invention is a non-melt-flowable TFE copolymer aqueous dispersion, and the redispersion sedimentation rate of the copolymer represented by the above formula (1) is 60% or less, and a content of perfluorooctanoic acid and its salts in the aqueous dispersion of less than 10 ppb is an important feature.
  • the dust-suppressing treatment agent composition of the present invention is mixed with a dust-generating substance, and the mixture is subjected to compression-shearing action at a temperature of about 20 to 200° C. to fibrillate the non-melt-flowable TFE copolymer.
  • the TFE polymer particles which are the solid content in the dust suppressing treatment agent composition, tend to settle.
  • the sedimented TFE polymer particles solidify and are difficult to redisperse by stirring or the like.
  • the redispersion sedimentation rate is 60% or less, it is possible to suppress the sedimented non-melt-flowable TFE copolymer particles from hardening, and to remarkably improve the redispersibility.
  • a small amount of the dust-suppressing treatment agent composition can be uniformly mixed with the dust-generating substance, so that generation of dust from the dust-generating substance can be efficiently suppressed.
  • the content of persistent perfluorooctanoic acid and its salts is less than 10 ppb, it is also excellent in environmental performance.
  • the dust-suppressing treatment agent composition of the present invention is excellent in dust-suppressing performance and redispersibility is confirmed by the centrifugal sedimentation test, centrifugal redispersion test, stationary sedimentation test, and stationary This is also clear from the results of the sedimentation redispersion test and the falling dust amount test.
  • the redispersion sedimentation rate of the non-melt-flowable TFE copolymer aqueous dispersion of the present invention is 60% or less.
  • the dust control treatment composition has a reduced amount of sedimentation compared to an aqueous dispersion of TFE polymer having a redispersion sedimentation rate of greater than 60%.
  • the dust suppressing treatment agent composition of the present invention has a redispersion sedimentation rate represented by the above formula (1) of 60% or less, preferably 50% or less, preferably 30%. % or less, it is clear that good redispersion can be achieved.
  • the non-melt-flowable TFE copolymer of the present invention is thought to have excellent sedimentation stability because it contains few rod-like particles that tend to sediment.
  • the redispersion sedimentation rate shown by the above formula (1) exceeds 60%, the sedimented non-melt-flowable TFE copolymer particles solidify and become difficult to redisperse.
  • the amount of the non-melt-flowable TFE copolymer particles dispersed in the dust suppressing treatment agent composition is reduced, and is equivalent to that before sedimentation.
  • more non-melt-flowable TFE copolymer aqueous dispersion is required.
  • the strongly solidified non-melt-flowable TFE copolymer cannot be used as a dust control agent and must be discarded. It is not preferable from an economical point of view because it wastes a large amount and generates a disposal cost.
  • the non-melt-flowable TFE copolymer used in the present invention comprises tetrafluoroethylene (TFE) and at least one comonomer selected from perfluoro(alkyl vinyl ether), (perfluoroalkyl)ethylene, and hexafluoropropylene. It is preferably a non-melt-flowable copolymer with.
  • the perfluoroalkyl group in (perfluoroalkyl)ethylene is preferably a perfluoroalkyl group having 1 to 10 carbon atoms, more preferably (perfluoroethyl)ethylene, ( It is at least one selected from perfluorobutyl)ethylene, (perfluorohexyl)ethylene, and (perfluorooctyl)ethylene. More preferred is (perfluorobutyl)ethylene.
  • the perfluoroalkyl group in the perfluoro(alkyl vinyl ether) is preferably a perfluoroalkyl group having 1 to 10 carbon atoms, more preferably perfluoro(methyl vinyl ether), It is at least one selected from perfluoro(ethyl vinyl ether) and perfluoro(propyl vinyl ether).
  • the amount of the comonomer in the non-melt-flowable TFE copolymer used in the present invention is 0.01 to 1.00% by mass, preferably 0.01 to 0.50% by mass, more preferably 0.01 to 0.50% by mass, based on TFE. It is contained in an amount of 01 to 0.30% by mass.
  • the content of the comonomer is 0.01 to 1.00% by mass, the stability of the aqueous dispersion is improved because there are few rod-shaped particles that tend to settle.
  • the content of the comonomer exceeds 1.00% by mass, the thermal stability is lowered, which is not preferable.
  • the content of the comonomer is less than 0.01% by mass, the redispersion sedimentation rate is inferior, which is not preferable.
  • the melting point of the non-melt-flowable TFE copolymer used in the present invention is 320-350°C, preferably 334-342°C. If the melting point is lower than 320° C., the comonomer content in the non-melt fluidity increases and fibrillation becomes difficult, which is not preferred.
  • the non-melt-flowable TFE copolymer used in the present invention is a copolymer that does not exhibit melt-moldability at temperatures above the melting point, and conforms to ASTM D1238 (372 ° C., load 5 kg) and is a temperature higher than the melting point. It is preferable that it is a copolymer whose MFR cannot be measured at .
  • Such a non-melt-flowable TFE copolymer is a copolymer different from the TFE copolymer that has melt-flowability and can be melt-molded.
  • the specific gravity (SSG) of the non-melt-flowable TFE copolymer is desirably 2.27 or less, preferably 2.22 or less, and more preferably 2.20 or less.
  • SSG value the lower the molecular weight, and the lower the SSG value, the higher the molecular weight. A high dust suppression effect can be obtained.
  • the non-melt-flowable TFE copolymer aqueous dispersion of the present invention is an aqueous dispersion in which fine particles (colloidal particles) of a high-molecular-weight non-melt-flowable TFE copolymer are dispersed.
  • the colloidal particles in the non-melt-flowable TFE copolymer aqueous dispersion have a particle size (d84) of 250 nm or less, preferably 50 to 250 nm, more preferably 50 to 225 nm when the cumulative volume percentage is 84%. Colloidal particles are preferred.
  • d84 is less than 50 nm, the effect of suppressing dust by the dust-generating substance may be lower than when d84 is within the above range.
  • the stability becomes low.
  • the particle size (d84) is 250 nm or less, unlike the case where the particle size (d50) is 250 nm or less, it means that there are no extremely large primary particles, and the sedimentation stability of the aqueous dispersion is excellent. means that
  • the concentration of the non-melt-flowable TFE copolymer in the non-melt-flowable TFE copolymer aqueous dispersion is not particularly limited, but is 10 to 80% by mass, preferably 15 to 80% by mass, or more. It is preferably in the range of 20 to 80% by mass.
  • the concentration of the non-melt-flowable TFE copolymer the better. If it is too high, the sedimentation stability (dispersion stability) may be impaired, which is not preferable.
  • the concentration of the non-melt-flowable TFE copolymer in the dust suppressing treatment agent composition of the present invention is preferably 10% by weight or more, particularly in the range of 20 to 80% by weight.
  • the concentration of the non-melt-flowable TFE copolymer is 5 mass. It is also possible to dilute the above-mentioned dust control treatment composition with water so that it becomes 10% or less.
  • the content of perfluorooctanoic acid and its salt in the non-melt-flowable TFE copolymer aqueous dispersion is less than 10 ppb, preferably less than 5 ppb, more preferably 0 ppb based on the mass of the aqueous dispersion. It is desirable to have Since perfluorooctanoic acid and its salts are difficult to decompose and have environmental impact, it is desired that their content be as low as possible.
  • the concentration of perfluorooctanoic acid and its salt in the non-melt-flowable TFE copolymer aqueous dispersion was measured by placing 10 ml of the non-melt-flowable TFE copolymer aqueous dispersion in a polyethylene container in a freezer at -20°C. After freezing to agglomerate the non-melt-flowable TFE copolymer and separating it from water, the contents of the polyethylene container were all transferred to a Soxhlet extractor, extracted with about 80 ml of methanol for 7 hours, and diluted to a volume. It can be calculated by measuring the sample liquid with a liquid chromatograph.
  • the method for preparing the non-melt-flowable TFE copolymer aqueous dispersion containing less than 10 ppb of perfluorooctanoic acid and its salt is not particularly limited, but the following method can be exemplified.
  • perfluorooctanoic acid and its salts are not used as polymerization agents during polymerization, and fluoromonoether acid (C 3 F 7 -0-CF ( The ammonium salt of CF 3 )COOH) and the ammonium salt of fluoropolyether acid (C 3 F 7 -O-[CF(CF 3 )CF 2 ]n-CF(CF 3 )COOH) were used to prepare the TFE copolymer.
  • fluoromonoether acid C 3 F 7 -0-CF
  • fluoropolyether acid C 3 F 7 -O-[CF(CF 3 )CF 2 ]n-CF(CF 3 )COOH
  • the non-melt-flowable TFE copolymer in the dust-suppressing treatment agent composition of the dust-generating substance is a non-melt-flowable TFE copolymer of TFE and the comonomer, which is redispersed.
  • the sedimentation rate is 60% or less, it becomes possible to obtain an excellent redispersion sedimentation rate, in addition to being able to fibrillate similarly to the TFE homopolymer and to obtain the dust suppressing effect.
  • the content of perfluorooctanoic acid and its salt in the non-melt-flowable TFE copolymer aqueous dispersion is less than 10 ppb, it also has excellent environmental performance.
  • the non-melt-flowable TFE copolymer aqueous dispersion used in the present invention may further contain an emulsion stabilizer in order to enhance the stability of the non-melt-flowable TFE copolymer aqueous dispersion.
  • Hydrocarbon anionic surfactants are preferred as emulsion stabilizers. Since this surfactant essentially forms a water-insoluble or sparingly soluble salt with calcium, aluminum and iron, which are soil components, pollution of rivers, lakes and groundwater caused by surfactants can be avoided. .
  • hydrocarbon-based anionic surfactants include higher fatty acid salts, higher alcohol sulfate salts, liquid fatty oil sulfate salts, fatty alcohol phosphate salts, dibasic fatty acid ester sulfonates, alkylaryl There are sulfonates and the like, especially polyoxyethylene alkylphenyl ether ethylene sulfonic acid (n of polyoxyethylene is 1 to 6, alkyl has 8 to 11 carbon atoms), alkylbenzene sulfonic acid (alkyl has 10 to 10 carbon atoms), 12) Na, K, Li and NH4 salts such as dialkyl sulfosuccinates (alkyl has 8-10 carbon atoms) impart high mechanical stability to non-melt-flowable TFE copolymer aqueous dispersions. is possible, and the non-melt-flowable TFE copolymer particles are prevented from aggregating due to high-speed agitation or the like, so it can be
  • the dust suppressing treatment method using the dust suppressing treatment agent composition of the present invention comprises mixing the dust suppressing agent composition of the present invention with a dust-generating substance, and heating the mixture at 20 to 200°C, preferably 50 to 150°C.
  • a compression-shearing action at a temperature of , and fibrillating the non-melt-flowable TFE copolymer in the composition
  • the generation of dust from dust-generating substances can be suppressed. That is, when the specific non-melt-flowable TFE copolymer used in the present invention is subjected to compression-shearing action under appropriate conditions as described above, it fibrillates in a spider web-like manner and becomes ultrafine fibers. It is considered that the dust-suppressing treated article treated with the dust-suppressing agent composition is dust-suppressed because the dust-generating substances are captured and aggregated by the cobweb-like fine fibers.
  • the dust-generating substance to be dust-inhibited using the dust-inhibiting agent composition of the present invention is an inorganic and/or organic dust-generating substance, and there are no particular restrictions on the substance, shape, and the like.
  • the dust-suppressing treatment agent composition of the present invention can also be effectively applied to dust-generating powdery substances as dust-generating substances.
  • Dust-producing substances that can be particularly preferably treated include, for example, cements such as Portland cement and alumina cement, slaked lime, quicklime powder, mineral powders such as calcium carbonate, dolomite, magnesite, talc, silica, and fluorite, Clay mineral powder such as kaolin and bentonite, metals such as iron and steel, slag powder by-produced in the manufacturing process of non-ferrous metals, coal, combustion ash powder such as garbage, gypsum powder, powdered metals, carbon black, activated carbon powder, metals
  • Ceramic powder such as oxides, pigments, and the like, that is, all dust-generating substances that generate dust when solid particulate matter scatters and floats in the air.
  • the amount of the dust-suppressing agent composition of the present invention added to the dust-generating substance depends on the type of dust-generating substance, particle size distribution, specific gravity (true specific gravity, apparent specific gravity), dust-suppressing treatment temperature, compression-shearing action to be applied. It can be appropriately set depending on the degree, the degree of dust suppression of the obtained dust-suppressed product, and the like.
  • As a guideline for the amount to be added for example, 0.001 to 1.0% by mass of the dust suppressing treatment agent composition is added to the dust-generating powdery substance in terms of the solid content of the non-melt-flowable TFE copolymer resin. , and preferably in the range of 0.005 to 0.50% by mass, dust generated from the dust-generating powdery substance can be suppressed.
  • the non-melt-flowable TFE copolymer does not harden firmly even after standing still for a long period of time. Since it has excellent properties (low redispersion sedimentation rate), it is possible to reduce the disposal cost, and it is also preferable from the economic point of view.
  • Dust-proofing treatment can also be applied to dust-generating substances that dislike moisture.
  • Japanese Patent Publication No. 52-32877 can be referred to.
  • Particle size (d84) at a cumulative volume percentage of 84% The particle size (d84) of the non-melt-flowable TFE copolymer particles, or the particle size of the TFE polymer particles, is measured using Microtrac UPA150 Model No. 9340 (manufactured by Nikkiso Co., Ltd.) was used for the measurement.
  • Standard specific gravity (SSG) Measured according to ASTM D-4894.
  • a non-melt-flowable TFE copolymer aqueous dispersion obtained by emulsion polymerization or a TFE polymer aqueous dispersion was adjusted to a concentration of 15% by mass using pure water. After that, about 750 ml of the non-melt-flowable TFE copolymer aqueous dispersion or the TFE polymer aqueous dispersion adjusted to the above concentration is placed in a polyethylene container (500 ml volume), and vigorously shaken by hand to agglomerate the solid content. separated. The separated solid was dried at 150° C. for 2 hours.
  • the mass ratio of the standard sample to the mass of the same volume of water at room temperature (23 ⁇ 1° C.) was taken as the standard specific gravity.
  • the average value of the standard specific gravities of the two samples was obtained and used as the standard specific gravity.
  • This standard specific gravity serves as a measure of the average molecular weight, and generally, the lower the standard specific gravity, the larger the molecular weight.
  • measurement samples were also prepared for resin powders with known PFBE contents (% by mass) (two points with PFBE contents of 0% by mass and 0.03% by mass). The infrared spectra of these samples were measured, and the absorbance ratio X was determined by the following formula (3).
  • Absorbance ratio X (C - B) / (A - B) (3)
  • C 875 cm -1 peak height (absorbance)
  • a calibration curve is created from the PFBE content (mass%) of two samples whose PFBE content (mass%) is known and the absorbance ratio X, and the PFBE content (mass%) of the sample is calculated from the absorbance ratio X of the sample. asked.
  • measurement samples were also prepared for resin powders with known PPVE contents (% by mass) (two points with PPVE contents of 0% by mass and 0.75% by mass). Infrared spectra of these samples were measured, and the absorbance ratio and absorbance ratio X1 were determined by the following equations (4) and (5).
  • measurement samples are prepared for resin powders with known HFP contents (% by mass) (three points with HFP contents of 0.06% by mass, 0.08% by mass, and 0.12% by mass). Infrared spectra of these samples were measured, and the absorbance ratio and absorbance ratio X2 were determined by the following equations (6) and (7).
  • Absorbance ratio X 2 (absorbance ratio of sample/absorbance ratio of known sample) x 0.42 ...
  • Solid content mass% Weigh less than 6 g of the non-melt-flowable TFE copolymer aqueous dispersion or the TFE polymer aqueous dispersion into a tared aluminum dish, and add the non-melt-flowable TFE copolymer aqueous dispersion, or The mass of the TFE polymer aqueous dispersion (mass before drying) was weighed (measured to four decimal places). After that, leave it for 2 hours in a dryer at 105 ° C. to remove moisture, bake at a constant temperature of 380 ° C. for 20 minutes and cool to room temperature, then weigh the mass (mass after drying) and use the following formula (8 ) to calculate the solid content mass %.
  • Solid content mass% [(mass after drying - tare mass of aluminum pan) / mass before drying] x 100 (8)
  • the measurement sample was measured using an input-compensated differential scanning calorimeter Diamond DSC (manufactured by PerkinElmer Japan Co., Ltd.), using an empty super clean aluminum sample pan as a reference material, from 200 ° C to 370 ° C at 10 ° C per minute.
  • the calorific value was measured while the temperature was raised.
  • the temperature at which the observed endothermic peak was maximum was taken as the melting point of the measurement sample (resin powder).
  • Centrifugal sedimentation test 15 g of a non-melt-flowable TFE copolymer aqueous dispersion or TFE polymer aqueous dispersion having the composition shown in Table 1 is placed in a centrifuge tube (manufactured by Corning, 15 ml centrifuge tube). Centrifugation was performed for 30 minutes at a temperature of 20° C. and a rotation speed of 3000 rpm using a centrifuge (manufactured by Kubota Corporation, table top cooling centrifuge 5500, angle rotor RA508).
  • Sedimentation rate X 1 /X 0 ⁇ 100 (9)
  • X 0 15 g of the TFE polymer aqueous dispersion shown in Comparative Example 1 was centrifuged with a centrifuge at a temperature of 20°C and a rotation speed of 3000 rpm for 30 minutes, and then solid content other than the solid content that had settled to the bottom of the centrifuge tube. It is the sedimentation ratio (%) of solids indicated by the following formula (10) when (liquid portion: supernatant and unsettled solids) is removed.
  • Redispersion sedimentation rate (%) X 3 /X 2 ⁇ 100 (1')
  • X 2 15 g of the aqueous dispersion of the TFE polymer shown in Comparative Example 1 was heated to 20°C, It is the solid content sedimentation ratio (%) shown by the following formula (2') when re-dispersed after centrifuging with a centrifuge at a rotation speed of 3000 rpm for 30 minutes.
  • X 3 15 g of the non-melt-flowable TFE copolymer aqueous dispersion shown in Examples, It is the sedimentation ratio (%) of solid content represented by the following formula (2′) when re-dispersed after centrifuging with a centrifuge at a temperature of 20° C. and a rotation speed of 3000 rpm for 30 minutes.
  • Solid sedimentation ratio after redispersion (%) (Solid sedimentation amount after redispersion) / (Solid content mass before centrifugation) x 100 ... (2')
  • Sedimentation rate X 5 /X 4 ⁇ 100 (11)
  • X 4 15 g of the TFE polymer aqueous dispersion shown in Comparative Example 1 was allowed to stand at room temperature for 30 days, 60 days, and 90 days after closing the mouth of the centrifuge tube, and then sedimented. Remove solids other than solids (liquid part: supernatant and unsettled solids), leave the centrifuge tube upside down for 30 minutes, and remove the liquid part. Minute sedimentation ratio (%) ).
  • Redispersion sedimentation rate X 7 /X 6 ⁇ 100 (13)
  • X 6 15 g of the TFE polymer aqueous dispersion shown in Comparative Example 1 was allowed to stand at room temperature for 30 days, 60 days, and 90 days after closing the mouth of the centrifuge tube, and then sedimented. After removing non-solid content (liquid portion: supernatant and unsettled solid content), leaving the centrifuge tube upside down for 30 minutes to further remove the liquid portion, and re-dispersing, the following formula ( 14) is the solid sedimentation ratio (%).
  • Drop dust generation test 200 g of the sample (dust-suppressed product) is allowed to fall naturally from the top inlet of a cylindrical container with an inner diameter of 39 cm and a height of 59 cm, and the amount of floating dust in the container at a height of 45 cm from the bottom (relative concentration (CPM: Counts per Minute) ) was measured with a scattered light digital dust meter. The amount of suspended dust is measured five times continuously for one minute after the sample is added, and the geometric mean value x (CPM) of the value obtained by subtracting the measured value (dark count) before the sample is added is taken as the "falling dust generation" of the sample. quantity.
  • the geometric mean value x was obtained by the following formula (15).
  • Example 1 Polymerization of non-melt-flowable TFE copolymer 60 g of paraffin wax, 2087 ml of deionized water, fluoromonoether acid (formula C 3 F 7 -0 12.03 g of ammonium salt of fluoropolyether acid ( C 3 F 7 -O-[CF(CF 3 )CF 2 ]n-CF(CF 3 )COOH). 1.0 g and 0.01 g of polyoxyethylene alkylphenyl ether were charged, and while heating to 80° C., the inside of the system was purged with nitrogen gas three times to remove oxygen, and then evacuated.
  • TFE tetrafluoroethylene
  • Example 2 A non-melt-flowable TFE copolymer aqueous dispersion was obtained in the same manner as in Example 1, except that the amount of PFBE was changed as shown in Table 1.
  • particle size (d84) at cumulative volume percentage of 84%, SSG, PFBE content, solid content mass, melting point, and perfluorooctanoic acid and its salts amount was measured.
  • a centrifugal sedimentation test and a centrifugal sedimentation redispersion test were conducted. The results are shown in Table 1 and FIG.
  • Example 4 Powdered quicklime containing 95.7% CaO and 1.6% MgO (through a 2.0 mm standard mesh sieve, 1.0 mm standard mesh sieve residue 17.3%, 600 ⁇ m standard mesh sieve residue 18.9%, 300 ⁇ m standard mesh sieve residue 18.1%, 150 ⁇ m standard mesh sieve residue 14.1%, 150 ⁇ m standard mesh sieve passage 31.6% powdered quicklime) 1,000 g in volume 5 liter small soil mixer, and while stirring at a rotation speed of 140 rpm, the non-melt-flowable TFE copolymer aqueous dispersion or TFE polymer aqueous dispersion prepared in Example 2 or Comparative Example 1 was added to the solid content mass.
  • a mass equivalent to 0.05 g in terms of conversion (0.005% by mass in solid content mass of the non-melt-flowable TFE copolymer or TFE polymer with respect to quicklime) was weighed, and the non-melt-flowable TFE copolymer aqueous The dispersion or TFE polymer aqueous dispersion was diluted with water so that the total amount of water and water contained in the dispersion was 100 g, and the dispersion in which the composition was dispersed was gradually added.
  • Example 5 and 6 Comparative Examples 3 and 4
  • the non-melt-flowable TFE copolymer aqueous dispersion or TFE polymer aqueous dispersion prepared in Example 2 or Comparative Example 1 was added in an amount shown in Table 3 (solid content mass% relative to the dust-generating substance).
  • a drop dust generation test was conducted on the obtained dust-suppressing treated material. Table 3 shows the results.
  • Examples 7-13 Polymerization of non-melt-flowable TFE copolymer 60 g of paraffin wax, 2087 ml of deionized water, fluoromonoether acid (formula C 3 F 7 -0 12.03 g of ammonium salt of fluoropolyether acid ( C 3 F 7 -O-[CF(CF 3 )CF 2 ]n-CF(CF 3 )COOH). 1.0 g and 0.01 g of polyoxyethylene alkylphenyl ether were charged, and while heating to 80° C., the inside of the system was purged with nitrogen gas three times to remove oxygen, and then evacuated.
  • the comonomer HFP or PPVE
  • TFE tetrafluoroethylene
  • Examples 14, 15, 21, 23, 24, 29, 30, 32-35 The dust-generating substances shown below and the non-melt-flowable TFE copolymer aqueous dispersions prepared in Examples 7 to 13 were added in the amounts shown in Table 5 or Table 6 (mass% of solid content relative to the dust-generating substances). Weigh a mass equivalent to , and use a dispersion diluted with water so that the total amount of water and water contained in the non-melt-flowable TFE copolymer aqueous dispersion is 100 g. A dust-suppressing treatment was obtained. A drop dust generation test was conducted on the obtained dust-suppressing treated material. The results are shown in Table 5 or Table 6.
  • Examples 16-20, 22, 25-28, 31 The dust-generating substances shown below and the non-melt-flowable TFE copolymer aqueous dispersions prepared in Examples 7 to 13 were added in the amounts shown in Table 5 or Table 6 (mass% of solid content relative to the dust-generating substances). Weigh a mass equivalent to , and use a dispersion diluted with water so that the total amount of water and water contained in the non-melt-flowable TFE copolymer aqueous dispersion is 35 g. A dust-suppressing treatment was obtained. A drop dust generation test was conducted on the obtained dust-suppressing treated material. The results are shown in Table 5 or Table 6.
  • the mass of the polymer + 100 g of water) was put into the mortar mixer, and the stirring of the mixer was stopped after 3 minutes from the start of stirring. After that, the quicklime in the mortar mixer was transferred to an enamel tray and left to cool for about 5 minutes to obtain a dust-suppressed product.
  • Ordinary Portland cement (64.3% CaO and 1.1% MgO , 20.5% SiO2, 5.1% Al2O3 , 3.1 % Fe2O3 and SO3 containing 2.0%) (2.0 mm standard mesh sieve, 1.0 mm standard mesh sieve, 600 ⁇ m standard mesh sieve, 300 ⁇ m standard mesh sieve, 150 ⁇ m standard mesh sieve residue 0.00 22%, 99.78% ordinary Portland cement passing through a standard mesh sieve of 150 ⁇ m) Dustproof treatment of a 9:1 mixture of ordinary Portland cement (hereinafter referred to as cement) and the powdered quicklime (Examples 16, 22, 25, 31): 450 g ⁇ 2 of cement was weighed, spread evenly on an enamel tray, and heated at 105° C.
  • cement ordinary Portland cement
  • powdered quicklime Examples 16, 22, 25, 31
  • Anhydrous gypsum (2.0 mm standard mesh sieve all through, 1.0 mm standard mesh sieve all through, 600 ⁇ m standard mesh sieve residue 0.13%, 300 ⁇ m standard mesh sieve residue 0.22%, Anhydrous gypsum with a 150 ⁇ m standard mesh sieve residue of 11.33% and a 150 ⁇ m standard mesh sieve passage of 88.31%) Dustproof treatment of anhydrite (Examples 17 and 26): 500 g ⁇ 2 of anhydrous gypsum were weighed, spread evenly on an enamel tray, and heated at 105° C. for one day.
  • 500 g of heated anhydride gypsum was weighed into a container of a mortar mixer, and the dispersion diluted with water (the mass of the non-melt-flowable TFE copolymer corresponding to the addition amount shown in Table 5 or Table 6 + 35 g of water ) is put into a mortar mixer and stirred at a low speed for 1 minute, 500 g of anhydride gypsum heated to 105 ° C. is added and stirred for 3 minutes, spread evenly on an enamel tray, and heated at 105 ° C. for 1 hour. A mixture was obtained. About 1 kg of the mixture was placed in a mortar and stirred with a pestle for 9 minutes to obtain a dust-suppressing treatment.
  • Ground granulated blast furnace slag (2.0 mm standard mesh sieve through, 1.0 mm standard mesh sieve through, 600 ⁇ m standard mesh sieve residue 0.02%, 300 ⁇ m standard mesh sieve residue 0 0.06%, granulated blast furnace slag with a 150 ⁇ m standard mesh sieve residue of 0.31% and a 150 ⁇ m standard mesh sieve passage of 99.61%)
  • Dust-proof treatment of ground granulated blast furnace slag (Examples 18 and 27): A dust-suppressing treated product was obtained in the same manner as the dust-proofing treatment of anhydrous gypsum, except that granulated granulated blast furnace slag was used.
  • Dolomite (2.0 mm standard mesh sieve through, 1.0 mm standard mesh sieve residue 0.06%, 600 ⁇ m standard mesh sieve residue 0.50%, 300 ⁇ m standard mesh sieve residue 3.44 %, Dolomite with 150 ⁇ m standard mesh sieve residue 8.20%, 150 ⁇ m standard mesh sieve passage 87.79%) Dustproof treatment of dolomite (Examples 19 and 28): 500 g ⁇ 2 of dolomite was weighed, spread evenly on an enamel tray, and heated at 105° C. for one day and night.
  • 500 g of heated dolomite was weighed into a container of a mortar mixer, and the dispersion diluted with the above water (the mass of the non-melt-flowable TFE copolymer corresponding to the addition amount shown in Table 5 or Table 6 + 35 g of water). is put into a mortar mixer and stirred at a low speed for 1 minute, 500 g of dolomite heated to 105 ° C. is added and stirred for 3 minutes, spread evenly on an enamel tray, heated at 105 ° C. for 1 hour to make the mixture Obtained. About 1 kg of the mixture was placed in a mortar mixer and stirred for 3 minutes to obtain a dust-suppressing product.
  • lignite powder was added in 3 portions of 1/4 each and mixed, then spread evenly on an enamel tray and heated at 105° C. for 1 hour to obtain a mixture.
  • About 500 g of the mixture was placed in a mortar and mixed with a pestle until the non-melt-flowable TFE copolymer was sufficiently fibrillated to obtain a dust-suppressing treatment.
  • the dust control agent composition of the present invention can be used in the fields of building materials, soil stabilizers, solidifying materials, fertilizers, landfill disposal of incinerated ash or hazardous substances, explosion-proof fields, cosmetics fields, and fillers for various plastics. It is suitably used in the field and the like to obtain a dust-restricted product of a dust-generating substance by subjecting the dust-generating substance to a dust-reducing treatment.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

La présente invention concerne une composition d'un agent de traitement d'élimination des poussières, pour éliminer les poussières d'un matériau produisant des poussières, la composition comprenant une dispersion aqueuse d'un copolymère de tétrafluoréthylène sans fluidité à l'état fondu, le taux de sédimentation par redispersion du copolymère étant de 60 % ou moins et la concentration de l'acide perfluorooctanoïque et d'un sel de ce dernier étant inférieure à 10 ppb par rapport à la masse de la dispersion aqueuse, en présentant ainsi un excellent effet d'élimination des poussières, une excellente re-dispersibilité des particules d'un copolymère de TFE sans fluidité à l'état fondu, c'est-à-dire la teneur en extrait sec de la composition d'agent de traitement d'élimination des poussières après abandon au repos pendant longtemps, et d'excellentes performances environnementales.
PCT/JP2022/044902 2021-12-06 2022-12-06 Composition d'un agent de traitement pour élimination des poussières WO2023106287A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997017382A1 (fr) * 1995-11-09 1997-05-15 Daikin Industries, Ltd. Poudre fine de polytetrafluoroethylene, sa fabrication et son utilisation
JP2010037365A (ja) * 2008-07-31 2010-02-18 Daikin Ind Ltd 含フッ素ポリマーの製造方法。
WO2015020100A1 (fr) * 2013-08-09 2015-02-12 ダイキン工業株式会社 Procédé d'analyse d'un article contenant un agent de traitement de surface contenant du fluor
JP2020189795A (ja) * 2019-05-21 2020-11-26 ダイキン工業株式会社 フルオロアルキルカルボン酸またはその塩の製造方法
JP2021042175A (ja) * 2019-09-12 2021-03-18 株式会社ニッペコ 抗菌・防カビ処理剤

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5050442B2 (ja) * 2006-07-12 2012-10-17 旭硝子株式会社 ポリテトラフルオロエチレン水性分散液
US9243080B2 (en) * 2012-11-30 2016-01-26 Daikin Industries, Ltd. Production method for polytetrafluoroethylene aqueous dispersion

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997017382A1 (fr) * 1995-11-09 1997-05-15 Daikin Industries, Ltd. Poudre fine de polytetrafluoroethylene, sa fabrication et son utilisation
JP2010037365A (ja) * 2008-07-31 2010-02-18 Daikin Ind Ltd 含フッ素ポリマーの製造方法。
WO2015020100A1 (fr) * 2013-08-09 2015-02-12 ダイキン工業株式会社 Procédé d'analyse d'un article contenant un agent de traitement de surface contenant du fluor
JP2020189795A (ja) * 2019-05-21 2020-11-26 ダイキン工業株式会社 フルオロアルキルカルボン酸またはその塩の製造方法
JP2021042175A (ja) * 2019-09-12 2021-03-18 株式会社ニッペコ 抗菌・防カビ処理剤

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