Elastic fiber treatment agent and use thereof
By using a treatment agent for elastic fibers of specific components, the problem of insufficient inhibition of flying flower adsorption in high-speed weaving is solved, and the yarn breakage rate and the production efficiency are improved.
Patent Information
- Application Number
- CN202380084601.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Priority Date
- 2023-04-05
- Filing Date
- 2023-11-27
- Publication Date
- 2025-07-18
AI Technical Summary
The existing treatment agent for elastic fibers has insufficient effect on suppressing the adsorption of flying flowers in high-speed post-processing process, resulting in frequent yarn suction port breakage and affecting production efficiency.
The treatment agent for elastic fibers containing specific base components and silicone resins is used. The base components include silicone oil, ester oil or hydrocarbon oil, the silanol group density is 0.1 mol% to 25.0 mol%, and the silanol group concentration of the silicone resin is 0.001 mmol/g to 0.10 mmol/g, and the organophosphate ester compound and the organic sulfonic acid compound are further added.
It significantly inhibits the adsorption of flying flowers, reduces the yarn breakage rate, improves production efficiency and braided substances, and is suitable for high-speed braiding processes.
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Abstract
Description
Technical Field
[0001] The present invention relates to a treating agent for elastic fibers and elastic fibers provided with the treating agent. Background Art
[0002] Elastic fibers are affected by the adhesiveness of the treatment agent on the fiber surface. In the post-processing step of interweaving the elastic fibers with cotton yarn, the flying fibers are adsorbed on the elastic fibers and blocked at the yarn suction port, and the yarn breaks at the yarn suction port, so there is a problem that cleaning is required every time. In order to solve these problems, for example, a polyurethane elastic fiber treatment agent containing a phosphite compound and a higher fatty acid magnesium salt has been proposed (Patent Document 1).
[0003] However, although these treatment agents have the effect of inhibiting the absorption of flying waste at the previous weaving speed, with the speed of post-processing steps in recent years and the thinning of elastic fibers (for example, below 22 dtex), the effect of inhibiting the absorption of flying waste has become insufficient, and sometimes frequent yarn breakages at the suction port cause a decrease in production efficiency.
[0004] Prior art literature
[0005] Patent Literature
[0006] Patent Document 1: Japanese Patent Application Laid-Open No. 2004-76187 Summary of the invention
[0007] Technical problem that the invention aims to solve
[0008] Therefore, an object of the present invention is to provide a processing agent for elastic fibers having excellent fly waste absorption suppressing properties.
[0009] Technical solutions to the problem
[0010] In view of the above-mentioned actual situation, the present inventors conducted intensive research on a treatment agent for elastic fibers having excellent fly waste absorption inhibition properties. As a result, they found that a specific treatment agent for elastic fibers containing a specific base component (A) and a silicone resin can solve the above-mentioned problems, thereby completing the present invention.
[0011] That is, the processing agent for elastic fibers of the present invention includes the following aspects.
[0012] <1> A treatment agent for elastic fibers, comprising: a base component (A), wherein the base component (A) contains at least one selected from silicone oil, ester oil and hydrocarbon oil; and an organic silicone resin (b), wherein the organic silicone resin (b) satisfies the following condition 1.
[0013] Condition 1: silanol group density is 0.1 mol% to 25.0 mol%
[0014] <2>The treating agent for elastic fibers according to <1>, wherein the weight average molecular weight of the above silicone resin (b) is 2,000 to 30,000.
[0015] <3>A treating agent for elastic fibers, which contains a base component (A) and a silicone resin (B), the above base component (A) contains at least one selected from silicone oil, ester oil and hydrocarbon oil, and the concentration of silanol groups in the treating agent for elastic fibers is 0.001 mmol / g to 0.10 mmol / g.
[0016] <4>The treating agent for elastic fibers according to any one of <1> to <3>, wherein the above treating agent for elastic fibers further contains at least one selected from organophosphate compounds and organic sulfonic acid compounds.
[0017] <5>The treating agent for elastic fibers according to any one of <1> to <4>, wherein the total content of sulfur element and phosphorus element detected from the treating agent by ICP emission spectrometry is 100 ppm to 5,000 ppm.
[0018] <6>An elastic fiber, which is obtained by applying the treating agent for elastic fibers according to any one of <1> to <5> to an elastic fiber main body.
[0019] <7>A method for manufacturing an elastic fiber, which includes: a step of applying the treating agent for elastic fibers according to any one of <1> to <5> to an elastic fiber main body.
[0020] Advantages of the Invention
[0021] The elastic fiber obtained by applying the treating agent for elastic fibers of the present invention has excellent fly-attachment inhibition property. Description of the Drawings
[0022] Figure 1 It is a schematic diagram for explaining a method for measuring the unwinding speed ratio.
[0023] Figure 2 It is a schematic diagram for explaining a method for measuring the knitting tension.
[0024] Figure 3 It is a schematic diagram for explaining a fly-attachment test method. Detailed Embodiments
[0025] The treating agent for elastic fibers of the first aspect of the present invention is a treating agent for elastic fibers containing a base component (A) and a silicone resin (b) satisfying the following Condition 1, and the base component (A) contains at least one selected from silicone oil, ester oil and hydrocarbon oil.
[0026] Condition 1: The silanol group density is 0.1 mol% to 25.0 mol%
[0027] The treating agent for elastic fibers in the second mode of the present invention contains a base component (A) and a silicone resin (B). The base component (A) contains at least one selected from silicone oil, ester oil, and hydrocarbon oil, and the silanol group concentration of the treating agent for elastic fibers is 0.001 mmol / g to 0.10 mmol / g.
[0028] The treating agents for elastic fibers will be described in detail below.
[0029] [Base component (A)]
[0030] The base component (A) contained in the treating agents for elastic fibers in the first and second modes contains at least one selected from silicone oil, ester oil, and hydrocarbon oil. The base component (A) is an essential component of the above-mentioned treating agent for elastic fibers and is a reagent for reducing the friction between fibers and metals.
[0031] From the aspect of the effect of reducing the friction between fibers and metals, the weight ratio of the base component (A) in the treating agents for elastic fibers in the first and second modes is preferably 10% by weight to 99.999% by weight. The upper limit of this weight ratio is more preferably 99% by weight, further preferably 90% by weight, and particularly preferably 80% by weight. On the other hand, the lower limit of this weight ratio is more preferably 20% by weight, further preferably 30% by weight, particularly preferably 50% by weight, and most preferably 60% by weight.
[0032] The base component (A) preferably contains at least one selected from silicone oil and mineral oil. When the base component (A) contains at least one selected from silicone oil and mineral oil, from the aspect of the effect of reducing the friction between fibers and metals, the total weight ratio of silicone oil and mineral oil in the base component (A) is preferably 10% by weight to 100% by weight. The upper limit of this weight ratio is more preferably 99% by weight, further preferably 90% by weight, and particularly preferably 80% by weight. On the other hand, the lower limit of this weight ratio is more preferably 20% by weight, further preferably 30% by weight, particularly preferably 50% by weight, and most preferably 60% by weight.
[0033] When the base component (A) contains silicone oil, from the aspects of the effect of reducing the friction between fibers and metals and the stability of the treating agent, the weight ratio of silicone oil in the base component (A) is preferably 10% by weight to 100% by weight. The upper limit of this weight ratio is more preferably 99% by weight, further preferably 90% by weight, and particularly preferably 80% by weight. On the other hand, the lower limit of this weight ratio is more preferably 20% by weight, further preferably 30% by weight, particularly preferably 50% by weight, and most preferably 60% by weight.
[0034] When the base component (A) contains mineral oil, considering the effect of reducing the friction between the fiber and the metal and the stability of the treatment agent, the weight ratio of the mineral oil in the base component (A) is preferably 10% by weight to 100% by weight. The upper limit of this weight ratio is more preferably 99% by weight, further preferably 90% by weight, and particularly preferably 80% by weight. On the other hand, the lower limit of this weight ratio is more preferably 20% by weight, further preferably 30% by weight, particularly preferably 50% by weight, and most preferably 60% by weight.
[0035] When the base component (A) contains ester oil, considering the aspect of suppressing the unwinding of the cheese (Japanese: チーズ), the weight ratio of the ester oil in the base component (A) is preferably 10% by weight to 100% by weight. The upper limit of this weight ratio is more preferably 99% by weight, further preferably 90% by weight, and particularly preferably 80% by weight. On the other hand, the lower limit of this weight ratio is more preferably 20% by weight, further preferably 30% by weight, particularly preferably 50% by weight, and most preferably 60% by weight.
[0036] As the silicone oil, as long as it is a linear organopolysiloxane, there is no particular limitation, and examples include: polydimethylsiloxane, polymethylphenylsiloxane, polymethylalkylsiloxane, etc., and one or more of them can be used. Considering the stability of the treatment agent, the kinematic viscosity of the silicone oil at 25 °C is preferably 2 to 100 mm 2 / s, more preferably 5 to 70 mm 2 / s, further preferably 5 to 50 mm 2 / s.
[0037] For the silicone oil, the average bonding amount of the siloxane bond (SiOR 1 R 2 : R 1 and R 2 each independently represents an organic group) is preferably 3 to 100, more preferably 7 to 60, and further preferably 7 to 50. R 1 、R 2The organic group is a hydrocarbon group having 1 to 24 carbon atoms, and examples thereof include methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl, isopentyl, hexyl, cyclopropyl, cyclohexyl, phenyl, benzyl, etc. Methyl and phenyl are particularly preferred. In addition, unreacted silanol groups, unreacted halogen groups, polymerization catalysts, cyclic siloxanes, etc. derived from the raw materials may also be included. Although not particularly limited, specific examples thereof include Shin-Etsu Chemical Co., Ltd.'s trade names KF-96-10cs, KF-96-20cs, KF-96-50cs, KF-96-100cs, KF-96-1000cs, KF-96-10,000cs, KF-50-100cs, KF-4003, KF-4917, Momentive Performance Materials Inc.'s trade names TSF451-5A, TSF451-10, TSF451-20, TSF451-30, TSF451-50, TSF451-100, TSF451-1000, TSF451-1M, Toray Dow Corning Co., Ltd.'s trade names SH200-10CS, SH200-20CS, SH200-50CS, SH510-100CS, Asahi Kasei Wacker Silicone Co., Ltd.'s trade names WACKER SILICONE FLUID AK10, WACKER SILICONE FLUID AK20, WACKER SILICONE FLUID AK50, etc., polydimethylsiloxane, polyalkylsiloxane, polyalkylphenylsiloxane, etc.
[0038] As the ester oil, as long as it is an ester of a monohydric alcohol and a monocarboxylic acid, an ester of a monohydric alcohol and a polycarboxylic acid, or an ester of a polyhydric alcohol and a monocarboxylic acid, there is no particular limitation, and one or more thereof can be used. As the monohydric alcohol, the monohydric aliphatic alcohols, aromatic alcohols, alicyclic alcohols, phenols, etc. described below can be used. Among them, monohydric aliphatic alcohols and aromatic alcohols are preferred.
[0039] The kinematic viscosity of the ester oil at 25 °C is preferably 2 to 100 mm 2 / s, more preferably 5 to 70 mm 2 / s, and still more preferably 5 to 50 mm 2 / s.
[0040] As the monohydric aliphatic alcohol, there is no particular limitation, and examples thereof include methanol, ethanol, propanol, butanol, pentanol, hexanol, heptanol, octanol, 2-ethylhexanol, 1-nonanol, 1-decanol, undecanol, lauryl alcohol, tridecanol, isotridecanol, myristyl alcohol, pentadecanol, 1-hexadecanol, palmityl alcohol, 1-heptadecanol, stearyl alcohol, oleyl alcohol, isostearyl alcohol, nonadecanol, 1-eicosanol, docosanol, 1-tetracosanol, nervonic alcohol, ceryl alcohol, etc.
[0041] Examples of the aromatic alcohol include phenol and benzyl alcohol.
[0042] Examples of the alicyclic alcohol include cyclooctanol, cyclododecanol, cyclohexanol, cycloheptanol, cyclopentanol, menthol, and the like.
[0043] As the monocarboxylic acid, the monobasic aliphatic carboxylic acid, aromatic carboxylic acid, and hydroxycarboxylic acid described below can also be used. Among them, the monobasic aliphatic carboxylic acid and aromatic carboxylic acid are preferred.
[0044] The above monocarboxylic acid is not particularly limited, and examples thereof include valeric acid, caproic acid, enanthic acid, octanoic acid, 2-ethylhexanoic acid, capric acid, lauric acid, myristic acid, pentadecanoic acid, palmitic acid, palmitoleic acid, margaric acid, stearic acid, oleic acid, isostearic acid, isooleic acid, linoleic acid, linolenic acid, arachidic acid, behenic acid, lignoceric acid, cerotic acid, benzoic acid, lactic acid, and the like.
[0045] The polycarboxylic acid is not particularly limited, and examples thereof include oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, fumaric acid, phthalic acid, trimellitic acid, pyromellitic acid, citric acid, isocitric acid, and the like.
[0046] The polyhydric alcohol is not particularly limited, and examples thereof include ethylene glycol, diethylene glycol, polyethylene glycol, propylene glycol, dipropylene glycol, polypropylene glycol, 1,3-propanediol, 1,4-butanediol, neopentyl glycol, 1,5-pentanediol, 3-methyl-1,5-pentanediol, 1,6-hexanediol, 1,9-nonanediol, 2-methyl-1,8-octanediol, cyclohexanediol, glycerin, diglycerin, triglycerin, tetraglycerin, sorbitol, trimethylolpropane, pentaerythritol, and the like.
[0047] As specific examples of the ester oil, there is no particular limitation. For example, the following can be cited: methyl caprate, methyl laurate, methyl oleate, methyl erucate, methyl levulinate, ethyl isostearate, ethyl octanoate, ethyl valerate, heptyl valerate, heptyl hexanoate, octyl hexanoate, cetyl octanoate, isooctyl laurate, isopropyl myristate, isopropyl palmitate, isostearyl palmitate, butyl stearate, octyl stearate, oleyl laurate, isotridecyl stearate, octyl stearate, isooctyl stearate, tridecyl stearate, isobutyl stearate, methyl oleate, isobutyl oleate, heptyl oleate, oleyl oleate, polyethylene glycol dilaurate, polyethylene glycol dimyristate, polyethylene glycol dioleate, polyethylene glycol distearate, polypropylene glycol dilaurate, polypropylene glycol dimyristate, polypropylene glycol dioleate, polypropylene glycol distearate, dicetyl oxalate, diisooctyl malonate, dilauryl succinate, diisodecyl adipate, isononyl adipate, dioctyl adipate, diisooctyl fumarate, diisooctyl phthalate, dioctyl phthalate, dinonyl phthalate, diisodecyl phthalate, di(undecyl) phthalate, triisooctyl trimellitate, triisobutyl trimellitate, triisodecyl trimellitate, triisostearyl trimellitate, glyceryl triisooctanoate, glyceryl trilaurate, glyceryl trimyristate, glyceryl trioleate, glyceryl tristearate, sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate, sorbitan monooleate, sorbitan trioleate, sorbitan tristearate, sorbitan sesquioleate, sorbitan trilaurate, sorbitan tristearate, sorbitan tripalmitate, etc.
[0048] As the hydrocarbon oil, there is no particular limitation, and it preferably contains at least one selected from mineral oil, poly-α-olefin, and Fischer-Tropsch synthesis oil.
[0049] As the mineral oil, there is no particular limitation, and examples thereof include machine oil, spindle oil, liquid paraffin, etc., and one or more thereof can be used. From the viewpoint of the stability of the treatment agent, the Saybolt universal viscosity of the mineral oil at 30 °C is preferably 30 seconds to 350 seconds, more preferably 35 seconds to 200 seconds, and further preferably 40 seconds to 150 seconds. As the mineral oil, from the viewpoint of reducing the generation of odor, liquid paraffin is preferred. Although not particularly limited, specific examples thereof include Semtol 40 OIL under the trade name of sonneborn company, Carnation (registered trademark) under the trade name of sonneborn company, Cosmo Pure Spin D, Cosmo Pure Spin E, Cosmo Pure Spin RC, Cosmo Pure Spin RB, Cosmo Neutral 100, Cosmo Neutral 150, Cosmo Neutral 350, Cosmo White P60, Cosmo White P70, Cosmo White P120, Cosmo White P200, Cosmo White P260, Cosmo White P350P, Cosmo Pure Safety 10, Cosmo Pure Safety 22, Cosmo Pure Safety 32, Cosmo SP10, SP15, Cosmo SP32, Cosmo SP52, product numbers NT-60, NT-100 of Fukkol (registered trademark) under the trade name of Fuji Kosan Co., Ltd., Ultra-S2, Ultra-S 3, Ultra-S 4, Ultra-S 6 under the trade name of S-OIL company, product numbers 3, 4, 4Plus, 6, 6Plus, 6J, 8, 8J of YUBASE (registered trademark) under the trade name of SK Lubricants company, product numbers W8, W32, G9, K8, S32 of Diana Freshia (registered trademark) under the trade name of Idemitsu Kosan Co., Ltd., product number Crystal N72 of ExxonMobil company, SUN 60N under the trade name of Nippon Oil Corporation, etc., such as machine oil, spindle oil, liquid paraffin.
[0050] As the poly-α-olefin, for example, substances synthesized from α-olefins such as ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene, 1-nonene, 1-decene, 1-undecene, 1-dodecene, 1-tridecene, 1-tetradecene, etc. can be cited. Specifically, product names PAO201, PAO401, PAO601, PAO801 of Nippon Steel & Sumikin Chemical Co., Ltd., product numbers 40, 60, 80 of Lipolube (registered trademark) under the trade name of Lion Specialty Chemicals Co., Ltd., etc. can be cited. From the viewpoint of obtaining good smoothness with respect to metals, the kinematic viscosity of the poly-α-olefin at 40 °C is preferably 5 to 100 mm2 / s, more preferably 7 to 60 mm 2 / s, further preferably 9 to 50 mm 2 / s.
[0051] Fischer-Tropsch synthetic oil is obtained by converting natural gas, coal, or biomass into syngas, then converting it into wax through the Fischer-Tropsch process, and further converting it into lubricating oil through hydroisomerization and dewaxing processes. The oil derived from natural gas is called GTL (gas-to-liquid), the oil derived from coal is called CTL (coal-to-liquid), and the oil derived from biomass is called BTL (biomass-to-liquid).
[0052] From the perspective of obtaining good smoothness relative to metals, the kinematic viscosity of Fischer-Tropsch synthetic oil at 40 °C is preferably 5 to 100 mm 2 / s, more preferably 7 to 60 mm 2 / s, further preferably 9 to 50 mm 2 / s. The kinematic viscosity of Fischer-Tropsch synthetic oil is measured according to JIS K 2283.
[0053] As Fischer-Tropsch synthetic oil, there is no particular limitation, and examples include: XHVI 3 manufactured by Shell Lubricants, XHVI 4 manufactured by Shell Lubricants, XHVI 5.2 manufactured by Shell Lubricants, XHVI 8 manufactured by Shell Lubricants, etc. One kind of Fischer-Tropsch synthetic oil can be used, or two or more kinds can be used in combination.
[0054] [Silicone resin (B)]
[0055] Silicone resin (B) is an organopolysiloxane with a three-dimensional structure. The organopolysiloxane contains at least one selected from T, DT, MQ, MDQ, MT, MTQ, MDT, and MDTQ as a constituent component and does not have fluidity at 25 °C. Here, M, D, T, and Q respectively represent R a R b R c SiO 1 / 2 (wherein, R a 、R b and R c are all hydrocarbon groups) units, R a R b SiO 2 / 2 (wherein, R a and R b are all hydrocarbon groups) units, RSiO 3 / 2 (wherein, R is a hydrocarbon group) units, and SiO 4 / 2 units.
[0056] As R, Ra , R b and R c The alkyl groups of R and R are alkyl groups having 1 to 24 carbon atoms, and examples thereof include methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl, isopentyl, hexyl, cyclopropyl, cyclohexyl, phenyl, benzyl, etc. Methyl, ethyl, propyl, butyl, pentyl, and phenyl are particularly preferred.
[0057] The silicone resin (b) contained in the treating agent for elastic fibers of the first mode is one that satisfies the following Condition 1 in the silicone resin (B).
[0058] Condition 1: The silanol group density is 0.1 mol% to 25.0 mol%
[0059] From the aspect of further exerting the effects of the present application, the upper limit of the silanol group density of the silicone resin (b) is more preferably 20.0 mol%, further preferably 15.0 mol%, and particularly preferably 10.0 mol%. On the other hand, the lower limit of the silanol group density is more preferably 0.5 mol%, further preferably 1.0 mol%, and particularly preferably 2.0 mol%.
[0060] The silanol group density means the ratio of the number of silanol groups to the number of silicon atoms in the amount of the silicone resin (b), based on the method described in the examples.
[0061] Examples of the silicone resin (b) contained in the treating agent for elastic fibers of the first mode and the silicone resin (B) contained in the treating agent for elastic fibers of the second mode include silicone resins such as MQ silicone resin, MQT silicone resin, T silicone resin, and DT silicone resin. From the aspect of exerting the effects of the present application, MQ silicone resin and MQT silicone resin are preferred. In addition, one of these may be used or two or more may be used in combination.
[0062] The weight average molecular weight of the silicone resin (b) contained in the treating agent for elastic fibers of the first mode and the silicone resin (B) contained in the treating agent for elastic fibers of the second mode is not particularly limited, and from the aspect of the stability of the treating agent, it is preferably 2,000 to 30,000. The upper limit of the weight average molecular weight is more preferably 28,000, further preferably 25,000, and particularly preferably 20,000. On the other hand, the lower limit of the weight average molecular weight is more preferably 5,000, further preferably 8,000, and particularly preferably 10,000. The method for measuring the weight average molecular weight of the silicone resin (B) and the silicone resin (b) is based on the method described in the examples.
[0063] In consideration of the effects of the present application obtained from the balance and the stability of the treatment agent, the weight ratio of the silicone resin (b) in the treatment agent for elastic fibers in the first mode is preferably 0.001% by weight to 20% by weight. The upper limit of this weight ratio is more preferably 8% by weight, further preferably 5% by weight, and particularly preferably 3% by weight. The lower limit of this weight ratio is more preferably 0.01% by weight, further preferably 0.05% by weight, and particularly preferably 0.1% by weight.
[0064] In consideration of the effects of the present application obtained from the balance and the stability of the treatment agent, the weight ratio of the silicone resin (B) in the treatment agent for elastic fibers in the second mode is preferably 0.001% by weight to 20% by weight. The upper limit of this weight ratio is more preferably 8% by weight, further preferably 5% by weight, and particularly preferably 3% by weight. The lower limit of this weight ratio is more preferably 0.01% by weight, further preferably 0.05% by weight, and particularly preferably 0.1% by weight.
[0065] [Organic phosphate compound]
[0066] The treatment agents for elastic fibers in the first mode and the second mode may further contain an organic phosphate compound. When the treatment agent contains an organic phosphate compound, the weight ratio of the organic phosphate compound in the treatment agent is not particularly limited, and is preferably 0.1% by weight to 10% by weight. If the weight ratio of the organic phosphate is within the above range, there is a tendency for excellent antistatic properties. The upper limit of this weight ratio is more preferably 5% by weight, further preferably 3% by weight, and particularly preferably 1% by weight. On the other hand, the lower limit of this weight ratio is more preferably 0.2% by weight, further preferably 0.4% by weight, and particularly preferably 0.5% by weight.
[0067] As an organophosphate compound, it is not particularly limited as long as it contains at least one or more hydrocarbon groups or oxyalkylene groups in the molecule. For example, hexyl phosphate, octyl phosphate, decyl phosphate, dodecyl phosphate, tetradecyl phosphate, hexadecyl phosphate, octadecyl phosphate, docosyl phosphate, tris(octacosyl) phosphate, octadecenyl phosphate, 2-ethylhexyl phosphate, isoheptyl phosphate, isooctyl phosphate, isononyl phosphate, isodecyl phosphate, isoundecyl phosphate, isododecyl phosphate, isotridecyl phosphate, isotetradecyl phosphate, isohexadecyl phosphate, isooctadecyl phosphate, tert-butyl phosphate, benzyl phosphate, octylphenyl phosphate, cyclohexyl phosphate, polyoxyethylene 5 mol addition hexadecyl ether phosphate, polyoxyethylene 15 mol addition hexadecyl ether phosphate, polyoxyethylene 7 mol addition polyoxypropylene 3.5 mol addition secondary alkyl ether phosphate, polyoxyethylene 2 mol polyoxypropylene 5 mol addition dodecyl phosphate, polyoxyethylene 3 mol addition secondary alkyl ether phosphate, polyoxyethylene 2 mol addition dodecyl ether phosphate, polyoxyethylene 4 mol addition phenol phosphate, etc. can be cited. One kind of organophosphate can be used or two or more kinds can be used in combination.
[0068] The organophosphate compound can be an alkali metal salt and / or an alkaline earth metal salt. As the alkali metal and alkaline earth metal that form a salt with the organophosphate compound, at least one selected from sodium, potassium, calcium, and magnesium is preferred, at least one selected from calcium and magnesium is more preferred, and magnesium is particularly preferred.
[0069] In addition, the organophosphate compound can be a secondary amine salt and / or a tertiary amine salt. Among the secondary amine salts of organophosphates and the tertiary amine salts of organophosphates, the secondary amine is dialkanolamine, N-alkyl-substituted alkanolamine, N,N-dialkyl-substituted amine, etc., and the tertiary amine is trialkanolamine, N-alkyl-substituted dialkanolamine, N,N-dipolyoxyalkylene-substituted alkylamine, N,N-dialkyl-substituted alkanolamine, N,N,N-trialkyl-substituted amine, N,N,N',N'-tetrapolyoxyalkylene-substituted alkyl diamine, etc. Specifically, it is dicyclohexylamine, distearylamine, dilaurylamine, dibutylamine, diisopropylamine, trioctylamine, trimethylamine, stearyldimethylamine, lauryldimethylamine, stearylpropanolamine, laurylethanolamine, diethanolamine, triethanolamine, tripropanolamine, N-methyldiethanolamine, butylethanolamine, dibutylethanolamine, octylbutanolamine, N,N,N',N'-tetrakis(2-hydroxypropyl)ethylenediamine, N,N,N',N'-tetrakis(2-hydroxybutyl)ethylenediamine, N,N,N',N'-tetrakis(2-hydroxypropyl)hexamethylenediamine, etc.
[0070] 〔Organic sulfonic acid compound〕
[0071] The treating agent for elastic fibers in the first mode and the second mode may further contain an organic sulfonic acid compound. When the treating agent contains an organic sulfonic acid compound, the weight ratio of the organic sulfonic acid compound in the treating agent is not particularly limited, and is preferably 0.1% by weight to 10% by weight. If the weight ratio of the organic phosphate ester is within the above range, there is a tendency for excellent antistatic properties. The upper limit of this weight ratio is more preferably 5% by weight, further preferably 3% by weight, and particularly preferably 1% by weight. On the other hand, the lower limit of this weight ratio is more preferably 0.2% by weight, further preferably 0.4% by weight, and particularly preferably 0.5% by weight.
[0072] As the above-mentioned organic sulfonic acid compound, as long as it is an organic sulfonic acid compound containing at least one or more hydrocarbon groups or oxyalkylene groups in the molecule, there is no particular limitation, and examples thereof include: alkane sulfonic acid, dialkyl sulfosuccinic acid, alkylbenzene sulfonic acid, alkylnaphthalene sulfonic acid, etc. Specifically, examples include: methanesulfonic acid, fluorosulfonic acid, octanesulfonic acid, benzenesulfonic acid, p-toluenesulfonic acid, dodecyl-6-sulfonic acid, tetradecyl-7-sulfonic acid, hexadecyl-8-sulfonic acid, octadecyl-9-sulfonic acid, branched nonylbenzene sulfonic acid, linear decylbenzene sulfonic acid, branched decylbenzene sulfonic acid, linear dodecylbenzene sulfonic acid, branched dodecylbenzene sulfonic acid, branched tridecylbenzene sulfonic acid, linear tetradecylbenzene sulfonic acid, branched tetradecylbenzene sulfonic acid, branched hexadecylbenzene sulfonic acid, bis(2-ethylhexyl) sulfosuccinic acid, bis(dodecyl) sulfosuccinic acid, etc. One kind of the organic sulfonic acid ester compound or two or more kinds thereof can be used in combination.
[0073] The organic sulfonic acid compound can be an alkali metal salt and / or an alkaline earth metal salt. As the alkali metal and alkaline earth metal forming a salt with the organic sulfonic acid compound, at least one selected from sodium, potassium, calcium, and magnesium is preferred, at least one selected from calcium and magnesium is more preferred, and magnesium is particularly preferred.
[0074] In addition, the organic sulfonic acid compound can be a secondary amine salt and / or a tertiary amine. Among the secondary amine salts of the organic sulfonic acid compound and the tertiary amine salts of the organic sulfonic acid compound, the secondary amine is dialkanolamine, N-alkyl-substituted alkanolamine, N,N-dialkyl-substituted amine, etc., and the tertiary amine is trialkanolamine, N-alkyl-substituted dialkanolamine, N,N-dipolyoxyalkylene-substituted alkylamine, N,N-dialkyl-substituted alkanolamine, N,N,N-trialkyl-substituted amine, N,N,N',N'-tetrapolyoxyalkylene-substituted alkyl diamine, etc. Specifically, it is dicyclohexylamine, distearylamine, dilaurylamine, dibutylamine, diisopropylamine, trioctylamine, trimethylamine, stearyldimethylamine, lauryldimethylamine, stearylpropanolamine, laurylethanolamine, diethanolamine, triethanolamine, tripropanolamine, N-methyldiethanolamine, butylethanolamine, dibutylethanolamine, octylbutanolamine, N,N,N',N'-tetrakis(2-hydroxypropyl)ethylenediamine, N,N,N',N'-tetrakis(2-hydroxybutyl)ethylenediamine, N,N,N',N'-tetrakis(2-hydroxypropyl)hexamethylenediamine, etc.
[0075] 〔Other components〕
[0076] From the aspect of improving the performance of smoothness and unwinding property, in the treating agent for elastic fibers of the first mode and the second mode, in addition to the above-described components, at least one other component selected from modified silicone, higher alcohol, polyol, organic amine, metal soap, nonionic surfactant, cationic surfactant, and anionic surfactant can be further contained. One or more than two kinds of other components can be used.
[0077] The above-mentioned modified silicone generally refers to those having a structure in which at least one reactive (functional) group or non-reactive (functional) group is bonded to at least one of the two terminals, single terminal, side chain, and two terminals of the side chain of polysiloxane such as dimethyl silicone (polydimethylsiloxane).
[0078] More specifically, as the above-mentioned modified silicone, examples include: alkyl-modified silicone such as modified silicone having a long-chain alkyl (alkyl having 6 or more carbon atoms, 2-phenylpropyl, etc.); ester-modified silicone which is a modified silicone having an ester bond; polyether-modified silicone which is a modified silicone having a polyoxyalkylene (such as polyoxyethylene, polyoxypropylene, polyoxyethyleneoxypropylene, etc.); amino-modified silicone which is a modified silicone having an aminopropyl group, N-(2-aminoethyl)aminopropyl group, etc.; methanol-modified silicone which is a modified silicone having an alcoholic hydroxyl group; epoxy-modified silicone which is a modified silicone having an epoxy group such as a glycidyl group or an alicyclic epoxy group; carboxyl-modified silicone which is a modified silicone having a carboxyl group; mercapto-modified silicone which is a modified silicone having a mercapto group, etc.
[0079] As the above-mentioned higher alcohols, there is no particular limitation, and linear and / or branched alcohols having 6 to 30 carbon atoms can be cited. As specific examples, there can be cited: linear alcohols such as hexanol, heptanol, octanol, nonanol, decanol, undecanol, dodecanol, tridecanol, tetradecanol, pentadecanol, hexadecanol, heptadecanol, octadecanol, nonadecanol, eicosanol, heneicosanol, docosanol, tricosanol, tetracosanol, pentacosanol, hexacosanol, heptacosanol, octacosanol, nonacosanol and triacontanol; branched-chain alkanols such as 2-ethylhexanol, 2-propylheptanol, 2-butyl octanol, 1-methylheptadecanol, 2-hexyl octanol, 1-hexylheptanol, isodecanol, isotridecanol, 3,5,5-trimethylhexanol; linear alkenols such as hexenol, heptenol, octenol, nonenol, decenol, undecenol, dodecenol, tridecenol, tetradecenol, pentadecenol, hexadecenol, pentadec-9-en-1-ol, hexadec-9-en-1-ol, heptadecenol, octadecenol, nonadecenol, eicosenol, docosenol, tetracosenol, pentacosenol, hexacosenol, heptacosenol, octacosenol, nonacosenol and triacosenol; branched-chain alkenols such as isohexenol, 2-ethylhexenol, isotridecenol, 1-methylheptadecenol, 1-hexylheptenol, isotridecenol and isooctadecenol, etc.
[0080] As specific examples of the above-mentioned polyhydric alcohols, glycerol, diglycerol, sorbitan, erythritol, pentaerythritol, trimethylolpropane, sorbitol and ditrimethylolpropane can be cited.
[0081] As the organic amine, as long as it is an organic amine containing at least one or more hydrocarbon groups or oxyalkylene groups in the molecule, there is no particular limitation. For example, there can be cited: laurylamine, myristylamine, cetylamine, stearylamine, oleylamine, diethylamine, dioctylamine, distearylamine, methyl stearylamine, polyoxypropylene-added laurylamine, polyoxyethylene-added laurylamine, polyoxyethylene-added stearylamine, polyoxyethylene-added oleylamine, monoethanolamine, diethylethanolamine, dibutylethanolamine, triethanolamine, lauryl ethanolamine, trioctylamine, dimethyllaurylamine, dimethylmyristylamine, dimethylstearylamine, etc.
[0082] As the above-mentioned metal soaps, monovalent, divalent or trivalent metal salts of fatty acids having 8 to 22 carbon atoms can be cited. As metal soaps, for example, there can be cited: calcium laurate, calcium palmitate, barium myristate, magnesium myristate, magnesium palmitate, magnesium laurate, magnesium stearate, magnesium 2-ethylhexanoate, zinc behenate, aluminum tribehenate, calcium stearate, calcium 2-ethylhexanoate, aluminum stearate, aluminum palmitate, barium stearate, zinc caprate, zinc stearate, etc. These metal soaps can be used singly or in combination of two or more.
[0083] As the above nonionic surfactant, there is no particular limitation. For example, there can be mentioned: polyoxyalkylene alkyl ethers having an alkyl group with 8 to 22 carbon atoms (the oxyalkylene is 1 to 20 moles, the oxyalkylene is oxyethylene and / or oxypropylene, random and / or block), sorbitan fatty acid esters, oxyalkylene adducts of sorbitan fatty acid esters (the oxyalkylene is 1 to 20 moles, the oxyalkylene is oxyethylene and / or oxypropylene, random and / or block), etc., alkylene oxide adducts of polyhydric alcohols, alkylphenols having an alkyl group with 6 to 22 carbon atoms, oxyalkylene adducts of alkylphenols having an alkyl group with 6 to 22 carbon atoms (the oxyalkylene is 1 to 20 moles, the oxyalkylene is oxyethylene and / or oxypropylene, random and / or block), fatty acid polyoxyalkylene glycol esters (the oxyalkylene is 1 to 20 moles, the oxyalkylene is oxyethylene and / or oxypropylene, random and / or block), etc. These nonionic surfactants can be used singly or in combination of two or more.
[0084] As the above cationic surfactant, there is no particular limitation. For example, there are the above-mentioned organic amines or their salts, and quaternary ammonium salts. Specifically, as the quaternary ammonium salts, there can be mentioned: didecyldimethylammonium salts, decyltrimethylammonium salts, dioctyldimethylammonium salts, octyltrimethylammonium salts, etc. These cationic surfactants can be used singly or in combination of two or more.
[0085] As the above anionic surfactant, as long as it is an anionic surfactant other than organic phosphate compounds and organic sulfonic acid compounds, there is no particular limitation. For example, there are alkyl sulfates and / or their salts, polyoxyethylene alkyl ether sulfates and / or their salts, polyoxyethylene alkyl ether acetates and / or their salts, etc. Specifically, there can be mentioned alkyl sulfates and / or their salts having an alkyl group with 1 to 20 carbon atoms, polyoxyethylene alkyl ether sulfates and / or their salts having an alkyl group with 6 to 22 carbon atoms, polyoxyethylene alkyl ether acetates and / or their salts having an alkyl group with 6 to 22 carbon atoms, etc. These anionic surfactants can be used singly or in combination of two or more.
[0086] [Treatment agent for elastic fiber]
[0087] For the treatment agents for elastic fibers in the first mode and the second mode, it can be considered that by making the organosilicon resin (B) have a specific silanol group density, or by making the silanol group concentration of the treatment agent for elastic fibers within a specific range, the adsorption of the treatment agent for elastic fibers on the yarn surface is appropriate, the adhesiveness on the surface of the elastic fibers after applying the treatment agent is suppressed, and the suppression of fly fiber adsorption is excellent.
[0088] From the aspect of workability, the kinematic viscosity at 30 °C of the treatment agent for elastic fibers in the first mode and the second mode is preferably 5 to 50 mm 2 / s, more preferably 5 to 40 mm 2 / s, more preferably 6 to 20 mm 2 / s.
[0089] When the treating agent for elastic fibers in the first mode and the second mode further contains at least one compound selected from organophosphate compounds and organic sulfonic acid compounds, from the aspect of antistatic properties, the total weight ratio of the organophosphate compound and the organic sulfonic acid compound in the treating agent is preferably 0.1% by weight to 10% by weight. The upper limit of this weight ratio is more preferably 5% by weight, further preferably 3% by weight, and particularly preferably 2% by weight. On the other hand, the lower limit of this weight ratio is more preferably 0.2% by weight, further preferably 0.3% by weight, and particularly preferably 0.5% by weight.
[0090] The concentration of silanol groups in the treating agent for elastic fibers in the second mode is 0.001 to 0.10 mmol / g. From the aspect of further exerting the effects of the present invention, the upper limit of this silanol group concentration is more preferably 0.09 mmol / g, further preferably 0.08 mmol / g, and particularly preferably 0.07 mmol / g. On the other hand, the lower limit of this silanol group concentration is more preferably 0.003 mmol / g, further preferably 0.005 mmol / g, and particularly preferably 0.008 mmol / g. The concentration of silanol groups in the treating agent for elastic fibers is based on the method described in the examples.
[0091] For the treating agent for elastic fibers in the first mode and the second mode, from the aspect of imparting appropriate adhesiveness after the treating agent and suppressing the adsorption of flying fluff, the total content of sulfur element and phosphorus element detected from the treating agent by ICP emission spectrometry is preferably 100 ppm to 5,000 ppm. The upper limit of this content is more preferably 4,500 ppm, further preferably 4,000 ppm, and particularly preferably 3,500 ppm. On the other hand, the lower limit of this content is more preferably 200 ppm, further preferably 300 ppm, and particularly preferably 400 ppm. The measuring method of the content of sulfur element and phosphorus element based on ICP emission spectrometry is based on the method described in the examples.
[0092] Regarding the manufacturing method of the treating agent for elastic fibers in the first mode and the second mode, there is no particular limitation, and a known method can be adopted. For example, it can be a method of pre-mixing several components and then mixing with other components, or a method of mixing all components at once. In addition, when the treating agent for elastic fibers of the present invention contains a metal salt of a higher fatty acid, it can be manufactured by mixing the pulverized metal salt of a higher fatty acid with a base component, etc., or by mixing a metal salt of a higher fatty acid in a base component, etc., and using a conventionally known wet pulverizer to pulverize it into a specified average particle size.
[0093] When the treating agent for elastic fibers contains other components, from the aspect of maintaining the fluidity during the use of the treating agent, the weight ratio of the other components in the total treating agent for elastic fibers is preferably 0.01% by weight to 15% by weight, more preferably 0.1% by weight to 13% by weight, and still more preferably 0.5% by weight to 10% by weight.
[0094] 〔Elastic fiber〕
[0095] The elastic fiber of the present invention is obtained by imparting the treating agent for elastic fibers of the present invention to the elastic fiber main body. The adhesion ratio of the treating agent for elastic fibers in the whole elastic fiber is not particularly limited, and is preferably 0.1% by weight to 15% by weight, and more preferably 0.5% by weight to 10% by weight. As a method for imparting the treating agent for elastic fibers of the present invention to the elastic fiber main body, there is no particular limitation, and a known method can be adopted.
[0096] The elastic fiber (elastic fiber main body) of the present invention is an elastic fiber using polyether-based polyurethane, polyester-based polyurethane, polyether ester elastomer, polyester elastomer, polyethylene elastomer, polyamide elastomer, etc., and its elongation rate is usually 300% or more.
[0097] As the elastic fiber of the present invention, there can be mentioned polyurethanes or polyurethane ureas formed by reacting PTMG, polyester diol with organic diisocyanate and then chain-extending with 1,4-butanediol, ethylenediamine, propanediamine, pentanediamine, etc. For example, a polyurethane urea elastic fiber can be produced as follows: Prepare polytetramethylene glycol (PTMG) with a molecular weight of 1000 to 3000 and diphenylmethane diisocyanate (MDI), and react them in a solvent such as dimethylacetamide or dimethylformamide at a PTMG / MDI = 1 / 2 to 1 / 1.5 (molar ratio), and chain-extend with diamines such as ethylenediamine and propanediamine to obtain a polyurethane urea polymer, and spin a 20% to 40% solution of the polyurethane urea polymer at a spinning speed of 400 to 1200 m / min by dry spinning. There is no particular limitation on the suitable fineness of the elastic fiber main body.
[0098] The elastic fiber main body of the present invention may also contain inorganic substances such as titanium oxide, magnesium oxide, hydrotalcite, zinc oxide, and divalent metal soaps. As the divalent metal soaps, there can be mentioned: calcium 2-ethylhexanoate, calcium stearate, calcium palmitate, magnesium stearate, magnesium palmitate, magnesium laurate, barium stearate, zinc caprate, zinc behenate, and zinc stearate, etc. One or more inorganic substances can be used.
[0099] When the elastic fiber main body contains an inorganic substance, the uniform unwinding property is sometimes poor. However, by applying the treating agent of the present invention to the elastic fiber main body, good uniform unwinding property can be achieved. Therefore, the treating agent for elastic fibers of the present invention is suitable for the case where the elastic fiber main body contains an inorganic substance. The content of the inorganic substance in the elastic fiber main body is not particularly limited, preferably 0.01% by weight to 5% by weight, more preferably 0.1% by weight to 3% by weight.
[0100] As the use of the elastic fibers of the present invention, processed yarns such as covered yarns such as core-sheath yarn (CSY), single covered yarn, ply yarn (PLY), air covered yarn, etc. can be used, or used as fabrics through circular knitting, tricot knitting, etc. In addition, for the purpose of imparting elasticity to products that require elasticity such as stockings, socks, underwear, swimsuits, etc., or outerwear such as jeans and suits for comfort, these processed yarns and fabrics are used. In addition, it is recently also applicable to disposable diapers.
[0101] Examples
[0102] Hereinafter, the present invention will be specifically described by way of examples and comparative examples, but the present invention is not limited to the examples described herein. It should be noted that "percentage (%)" and "parts" shown in the following examples represent "wt%" and "parts by weight" unless otherwise specified. It should be noted that in the examples and comparative examples, the evaluation of each property of the treating agent for elastic fibers and the components used in the treating agent for elastic fibers was carried out according to the following methods.
[0103] (Unwinding speed ratio)
[0104] In Figure 1 , a bobbin (1) of fibers to which the treating agent has been applied is provided on the unwinding side of the unwinding speed ratio measuring machine, and a winding side paper tube (2) is provided. After setting the winding speed to a constant speed, rollers (3) and (4) are started simultaneously. In this state, almost no tension is applied to the yarn (5), so the yarn adheres to the bobbin without separating, and the unwinding point (6) is in the state shown in Figure 1 . By changing the unwinding speed, the unwinding point (6) of the yarn (5) from the bobbin is changed, so the unwinding speed is set so that this point coincides with the contact point (7) between the bobbin and the roller. The unwinding speed ratio is calculated by the following formula. The smaller this value, the better the unwinding property.
[0105] For the measured values, the anti-sticking property is judged by the following index, and values of ○ or above are regarded as qualified.
[0106] Unwinding speed ratio (%) = ((winding speed - unwinding speed) / unwinding speed) × 100
[0107] (Index)
[0108] ◎: When the unwinding speed ratio of the inner layer part is less than 100.
[0109] ○: When the unwinding speed ratio of the inner layer part is 100 or more and less than 130.
[0110] △: When the unwinding speed ratio of the inner layer part is 130 or more and less than 150.
[0111] ×: When the unwinding speed ratio of the inner layer part is 150 or more.
[0112] (Weaving tension)
[0113] In Figure 2 , the elastic yarn (9) longitudinally drawn from the cheese (8) passes through the compensator (10), via the roller (11), the knitting needle (12), via the roller (14) mounted on the U-shaped gauge (13), and is connected to the speedometer (15) and the take-up roller (16). The rotational speed of the take-up roller is adjusted so that the traveling speed in the speedometer (15) reaches a constant speed (10 m / min, 100 m / min), and it is wound on the take-up roller. The weaving tension at this time is measured using the U-shaped gauge (13), and the friction (g) between the fiber / knitting needle is measured.
[0114] For the measured values, the high-speed smoothness is judged using the following indices, and values of 〇 or more are regarded as qualified.
[0115] (Index)
[0116] ◎: The weaving tension value at 10 m / min is less than 15, and the weaving tension value at 100 m / min is less than 15
[0117] ○: The weaving tension value at 10 m / min is less than 15, and the weaving tension value at 100 m / min is 15 or more and less than 20
[0118] △: The weaving tension value at 10 m / min is less than 15, and the weaving tension value at 100 m / min is 20 or more and less than 25
[0119] ×: The weaving tension value at 10 m / min is 15 or more, or the weaving tension value at 100 m / min is 25 or more
[0120] (Flying lint adsorption test method)
[0121] In Figure 3 , the elastic yarn is released from the cheese (17) at a speed of 20 m / min, passes through the compensator (18), from the roller (19) via the flying lint suction port (20) and is wound by the take-up roller (21) at a speed of 80 m / min. The cotton yarn (22) is wound from the guide (23) via the roller (24) and the knitting needle (25) by the take-up roller (26) at a speed of 80 m / min.
[0122] Fly-ash is generated by twisting cotton yarn once between the roller (24) and the knitting needle (25) and rubbing them against each other. Measure the weight of the fly-ash accumulated at the yarn suction port when the elastic fiber travels for 60 minutes. The elastic fiber and the cotton yarn used were obtained by conditioning for 3 days in an atmosphere of 20 °C and 45% RH. The measurement atmosphere is carried out at 20 °C and 45% RH. The diameter of the yarn suction port is 0.2 mm, the length is 10 mm, and its material is alumina.
[0123] For the measured values, judge the fly-ash adsorption resistance with the following indicators, and regard those above 〇 as qualified.
[0124] (Indicator)
[0125] ◎: The weight of fly-ash is less than 0.5 mg
[0126] ○: The weight of fly-ash is 0.5 mg or more and less than 1.5 mg
[0127] △: The weight of fly-ash is 1.5 mg or more and less than 5.0 mg
[0128] ×: The weight of fly-ash is 5.0 mg or more
[0129] (Silanol group density)
[0130] Perform solid 29Si NMR measurement on the silicone resin, and set the peak area values of the Q1 structure, Q2 structure, Q3 structure, and Q4 structure calculated by waveform separation based on the obtained spectrum as S Q1 、S Q2 、S Q3 、S Q4 , and calculate the silanol group density from the following formula.
[0131] It should be noted that the Q1 structure to Q4 structure respectively represent the structures shown in the following general formula 1 to general formula 4. The Q1 structure has a peak around -70 to -84 ppm, the Q2 structure has a peak around -85 to -95 ppm, the Q3 structure has a peak around -96 to -103 ppm, and the Q4 structure has a peak around -104 to -123 ppm.
[0132] Silanol group density (mol%) = (3 × S Q1 + 2 × S Q2 + S Q3 ) / (S Q1 + S Q2 + S Q3 + S Q4 ) × 100
[0133] [Chemical formula 1]
[0134]
[0135] [Chemistry 2]
[0136]
[0137] [Chemistry 3]
[0138]
[0139] [Chemistry 4]
[0140]
[0141] (Method for determining phosphorus content in treatment agent based on ICP emission spectroscopy)
[0142] (1) Pretreatment
[0143] 5 g of the elastic fiber treatment agent was weighed in a platinum crucible, carbonized on an electric heater, and then 4 ml of sulfuric acid (for harmful metal determination) was added and ashed in an electric furnace. Finally, 0.5 ml of nitric acid (for harmful metal determination) and ultrapure water were added to make a fixed volume of 50 ml to prepare a test sample.
[0144] (2) Calibration curve
[0145] A 10 ppm standard solution and a 100 ppm standard solution with known phosphorus content, which were adjusted in advance, were respectively supplied to ICP (measurement equipment name: ICPS-8100 manufactured by Shimadzu Corporation, ICP emission spectrometer) to prepare a calibration curve (Japanese: 検量線).
[0146] (3) Determination
[0147] The measurement sample prepared in (1) was subjected to ICP (measurement instrument name: ICPS-8100 manufactured by Shimadzu Corporation, ICP emission spectrometer), and the content of phosphorus in the elastic fiber treatment agent was measured using the calibration curve prepared in (2).
[0148] (Method for determining sulfur content in treatment agent based on ICP emission spectroscopy)
[0149] (1) Pretreatment
[0150] 5 g of the elastic fiber treatment agent was weighed in a platinum crucible, carbonized on an electric heater, and then 4 ml of sulfuric acid (for harmful metal determination) was added and ashed in an electric furnace. Finally, 0.5 ml of nitric acid (for harmful metal determination) and ultrapure water were added to make a fixed volume of 50 ml to prepare a test sample.
[0151] (2) Calibration curve
[0152] Prepare a calibration curve by supplying a 10 ppm standard solution and a 100 ppm standard solution with a known sulfur element content that has been pre-adjusted to an ICP (measurement device name: ICPS-8100 manufactured by Shimadzu Corporation, ICP emission spectrometer).
[0153] (3) Measurement
[0154] Supply the measurement sample prepared in (1) above to an ICP (measurement instrument name: ICPS-8100 manufactured by Shimadzu Corporation, ICP emission spectrometer), and use the calibration curve prepared in (2) above to measure the sulfur element content in the treatment agent for elastic fibers.
[0155] (Weight-average molecular weight)
[0156] In the present invention, the weight-average molecular weight of the silicone resin is the value measured by gel permeation chromatography (GPC) under the following conditions.
[0157] Measurement device: HLC-8320GPC manufactured by Tosoh Corporation
[0158] Column: TSKgel4000HXL, TSKgel3000HXL, TSKgel2000HXL, TSKgel1000HXL manufactured by Tosoh Corporation
[0159] Detector: RI (differential refractometer)
[0160] Data processing: GPC workstation EcoSEC-WS manufactured by Tosoh Corporation
[0161] Measurement conditions: Column temperature 40 °C
[0162] Solvent: Tetrahydrofuran
[0163] Flow rate: 0.35 ml / min
[0164] Standard: Monodisperse polystyrene
[0165] Sample: A sample (100 μl) obtained by filtering a tetrahydrofuran solution with a resin solid content of 0.2 mass% in terms of resin solid content through a microfilter
[0166] (Silanol group concentration)
[0167] Measure the absorbance of the absorption band at 4200 - 4800 cm -1 or 6800 - 7400 cm -1 using an IR (infrared spectrophotometer), and compare the obtained absorbance with the absorbance of the treatment agent for elastic fibers with a known silanol group concentration, thereby calculating the silanol group concentration (mmol / g).
[0168] [Examples 1 - 16 and Comparative Examples 1 - 8]
[0169] (Adjustment of Spinning Dope)
[0170] Polytetramethylene ether glycol with a number - average molecular weight of 2000 was reacted with 4,4'-diphenylmethane diisocyanate at a molar ratio of 1:2. Then, chain extension was carried out using a dimethylformamide solution of 1,2 - diaminopropane to obtain a dimethylformamide solution with a polymer concentration of 27%. The viscosity at 30°C was 1500 mPa·s.
[0171] The polyurethane spinning dope was ejected into a N₂ gas stream at 190°C for dry spinning. For the moving yarn during spinning, a finishing agent (the blending amounts in the table are in weight %) made of the components described in Tables 2 - 4 and having a content of 6% by weight relative to the fiber was applied using an oiling roller, and then wound around a bobbin at a speed of 500 m per minute to obtain a 44 dtex monofilament cheese (winding amount 400 g). The obtained cheese was placed in an atmosphere of 35°C and 50% RH for 48 hours for evaluation. The evaluation results of the oil agent performance are shown in Tables 2 - 4. It should be noted that the components used in Tables 2 - 4 are as described below.
[0172] (Base Component (A))
[0173] a - 1: Dimethyl silicone (Japanese: ジメチルシリコーン) 10 mm 2 / s
[0174] a - 2: Dimethyl silicone 20 mm 2 / s
[0175] a - 3: Liquid paraffin 60 seconds
[0176] a - 4: Liquid paraffin 40 seconds
[0177] a - 5: 2 - Ethylhexyl stearate
[0178] As the silicone resin, the components described in Table 1 were used.
[0179] It should be noted that among the silicone resins in Table 1, those that meet Condition 1 are marked as 〇, and those that do not meet Condition 1 are marked as ×.
[0180] [Table 1]
[0181]
[0182] (Other Component (X))
[0183] x - 1: Magnesium stearate (average particle size 0.5 μm, needle - shaped (1:5))
[0184] x-2: Polyether-modified silicone
[0185] x-3: Isostearyl alcohol
[0186] x-4: Isotridecyl phosphate
[0187] x-5: Di-2-ethylhexyl sulfosuccinate sodium
[0188] [Table 2]
[0189]
[0190] [Table 3]
[0191]
[0192] [Table 4]
[0193]
[0194] As can be seen from Tables 2 to 4, in the case of Examples 1 to 16, the treating agent for elastic fibers of the first mode or the second mode of the present invention is used, so that the fly-adsorption inhibitory property of the wound yarn body is excellent.
[0195] On the other hand, since the treating agents for elastic fibers in Comparative Examples 1 to 7 use a treating agent for elastic fibers that does not contain the silicone resin (b) or the concentration of the silanol group is not 0.001 to 0.10 mmol / g, the fly-adsorption inhibitory property, which is the problem of the present application, is poor.
[0196] Industrial applicability
[0197] By using the treating agent of the present invention, elastic fibers with excellent fly-adsorption inhibitory property can be manufactured, so that the defective rate of the wound yarn body can be reduced, the operating rate of the knitting machine can be increased, and the quality of the knitted fabric can be improved.
[0198] Symbol description
[0199] 1 Bobbin
[0200] 2 Winding paper tube
[0201] 3 Roller
[0202] 4 Roller
[0203] 5 Traveling yarn strand
[0204] 6 Unwinding point
[0205] 7 Contact point between the bobbin and the roller
[0206] 8 Bobbin
[0207] 9 Elastic yarn
[0208] 10 Compensator
[0209] 11 Roller
[0210] 12 Knitting Needle
[0211] 13 U - gauge
[0212] 14 Roller
[0213] 15 Speedometer
[0214] 16 Take - up Roller
[0215] 17 Bobbin
[0216] 18 Compensator
[0217] 19 Roller
[0218] 20 Yarn Suction Port
[0219] 21 Take - up Roller
[0220] 22 Cotton Yarn
[0221] 23 Guide
[0222] 24 Roller
[0223] 25 Knitting Needle
Claims
1. A treating agent for elastic fibers, characterized in that, Comprising: a base component (A), the base component (A) comprising at least one selected from silicone oils, ester oils, and hydrocarbon oils; and a silicone resin (b), the silicone resin (b) satisfying the following Condition 1, Condition 1: The silanol group density is 0.1 mol% to 25.0 mol%.
2. The treating agent for elastic fibers according to claim 1, wherein the weight average molecular weight of the silicone resin (b) is 2,000 to 30,000.
3. A treating agent for elastic fibers, characterized in that the treating agent for elastic fibers contains a base component (A) and a silicone resin (B), the base component (A) comprising at least one selected from silicone oils, ester oils, and hydrocarbon oils, and the silanol group concentration of the treating agent for elastic fibers is 0.001 mmol / g to 0.10 mmol / g.
4. The treating agent for elastic fibers according to any one of claims 1 to 3, wherein the treating agent for elastic fibers further contains at least one selected from organophosphate compounds and organic sulfonic acid compounds.
5. The treating agent for elastic fibers according to any one of claims 1 to 4, wherein the total content of sulfur element and phosphorus element detected from the treating agent by ICP emission spectrometry is 100 ppm to 5,000 ppm.
6. An elastic fiber, characterized in that it is obtained by imparting the treating agent for elastic fibers according to any one of claims 1 to 5 to an elastic fiber main body.
7. A method for manufacturing an elastic fiber, characterized in that, Comprising: a step of imparting the treating agent for elastic fibers according to any one of claims 1 to 5 to an elastic fiber main body.
Citation Information
Patent Citations
Treatment agent for polyurethane elastic fiber and polyurethane elastic fiber coated with said treatment agent
JP2004076187A