JP3988123B2 - Polyurethane elastic fiber and method for producing the same - Google Patents

Description

【０１０７】
【表２】

【０１０８】
【発明の効果】
以上説明した本発明のポリウレタン系弾性繊維は、後加工工程で使用する際、ガイド類へスカムの脱落、蓄積を防止するため安定操業ができ、得られる編物、織物等の品質を優れたものとすることができるという効果がある。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a polyurethane-based elastic fiber and a method for producing the same.
[0002]
More specifically, when used in a post-processing step, the polyurethane elastic fiber capable of stably unwinding the yarn from the package and having excellent quality of the resulting knitted fabric, woven fabric, etc. It relates to the manufacturing method.
[0003]
[Prior art]
Polyurethane-based elastic fibers have large elongation and elongation recovery force, and are used for applications such as swimwear that require stretchability and fit due to their excellent elastic properties.
[0004]
However, since the elongation when a certain tensile stress is applied is large, the fibers are easily stretched due to the frictional resistance with the guides in the post-processing step, and spots such as the knitted fabric, the woven fabric, etc. are pulled.
[0005]
In addition, since polyurethane-based elastic fibers have high adhesiveness, the yarns in the package tend to stick together, making it difficult to unwind the yarn from the package.
[0006]
Various processing agents and additives are used to reduce the frictional resistance and adhesiveness with such guides.
[0007]
JP-A-42-8438, JP-A-2-127570, and JP-A-8-74179 disclose polydimethylsiloxane containing magnesium stearate as such a treating agent. It was hard to say that the unraveling property of the article was sufficiently improved.
[0008]
Furthermore, the conventional treatment agent containing magnesium stearate has a problem that the yarn rubs against the guides at a high speed, so that the scum drops and accumulates on the guides, causing trouble such as yarn breakage. It was.
[0009]
[Problems to be solved by the invention]
An object of the present invention is to provide a polyurethane-based elastic fiber that can be stably operated when used in a post-processing step, and can improve the quality of products such as knitted fabrics and woven fabrics obtained. is there.
[0010]
[Means for Solving the Problems]
The polyurethane elastic fiber of the present invention employs the following means in order to solve the above problems.
[0011]
That is, a treatment agent containing metal soap and having impurities of 50 ppm or less is applied. And the impurity is an inorganic salt containing at least one of nitrogen, phosphorus, sulfur, and chlorine. This is a polyurethane-based elastic fiber.
[0012]
Moreover, in order to solve the said subject, the manufacturing method of the polyurethane-type elastic fiber of this invention employ | adopts the following means.
[0013]
That is, a treatment agent containing metal soap and substantially free of impurities is applied. And the impurity is an inorganic salt containing at least one of nitrogen, phosphorus, sulfur, and chlorine. This is a method for producing a polyurethane-based elastic fiber.
[0014]
DETAILED DESCRIPTION OF THE INVENTION
The polyurethane elastic fiber of the present invention is provided with a treatment agent containing metal soap.
[0015]
If the treating agent used in the present invention does not contain metal soap, there is a problem that it is difficult to unwind the wound yarn from the package.
[0016]
Such metal soaps include stearic acid, palmitic acid, myristic acid, aicosanoic acid, docosanoic acid, lauric acid, 12-hydroxystearic acid, arachidic acid, behenic acid, octanoic acid, tall oil fatty acid and other fatty acids, abietic acid, neoabieticin Acids, d-pimalic acid, iso-d-pimalic acid, podocarpic acid, agatendicarboxylic acid, benzoic acid, cinnamic acid, p-oxycinnamic acid, diterpenic acid and other resin acids or alkali salts such as naphthenic acid Metal salts or mixed salts thereof are preferred.
[0017]
As the metal species in the metal salt, aluminum, calcium, zinc, magnesium, silver, barium, beryllium, cadmium, cobalt, chromium, copper, iron, mercury, manganese, nickel, lead, tin, titanium and the like are preferable.
[0018]
The metal soap used in the present invention is preferably a fatty acid metal salt, particularly preferably magnesium stearate or calcium stearate.
[0019]
The treatment agent used in the present invention preferably contains a smoothing agent, an antistatic agent, a dispersant and the like in addition to the metal soap.
[0020]
Smoothing agents include paraffinic hydrocarbons such as mineral oil, coconut oil, beef tallow, palm oil, castor oil, rapeseed oil and other natural oils, lauryl oleate, neopentyl dilaurate, oleyl oleate, dioleyl adipate, 2-ethylhexyl stearate. Aliphatic esters such as acrylate, isopropyl myristate, isopropyl palmitate, normal butyl stearate, isolauryl oleate, neopentyl glycol dioleate, trimethylolpropane tri-2-ethylhexanoate, pentaerythritol tetrapelargonate, siloxane As units, 1) polydimethylsiloxane composed of dimethylsiloxane units, 2) polydialkylsiloxanes composed of dimethylsiloxane units and dialkylsiloxane units containing an alkyl group having 2 to 4 carbon atoms. Emissions acids, 3) silicone oil polysiloxanes etc. consisting of dimethylsiloxane units and methylphenylsiloxane units is preferably used.
[0021]
In the present invention, the smoothing agent has a viscosity of 5 × 10 5 at 25 ° C. from the viewpoint of reducing handleability and running friction with guides. ^-6 ~ 50x10 ^-6 m ² / S is preferred. Such a viscosity can be measured by the method described in JIS-K2283 (crude oil and petroleum products-kinematic viscosity test method and viscosity index calculation method).
[0022]
As the antistatic agent, anionic surfactants such as alkyl sulfates, fatty acid soaps, alkyl sulfonates, and alkyl phosphates are preferably used.
[0023]
As the dispersant, silicone resin, polyether-modified silicone, carbinol-modified silicone, carboxyl-modified silicone, amino-modified silicone, amide-modified silicone, carboxyamide-modified silicone, mercapto-modified silicone, organic carboxylic acid, etc. are preferably used alone or as a mixture. Is done.
[0024]
In addition, the treatment agent used in the present invention contains, as necessary, components usually used in a synthetic fiber treatment agent such as a binder, an ultraviolet absorber, an antioxidant, a preservative, and a wettability improver. This is also preferably done. The contents of these metal soaps, smoothing agents, antistatic agents and the like are preferably determined appropriately according to the purpose.
[0025]
The treating agent used in the present invention has an impurity content of 50 ppm or less.
[0026]
When the impurity exceeds 50 ppm, there is a problem that scum drops and accumulates in the guides.
[0027]
An impurity means things other than the component contained in order to make processing agents, such as said metal soap, a smoothing agent, an antistatic agent, a dispersing agent, exhibit a predetermined effect.
[0028]
Impurities are considered to be by-produced in the manufacturing process of the metal soap and smoothing agent used, or mixed in during the manufacturing process of the treating agent for synthetic fibers.
[0029]
For example, the metal soap is produced by a direct method in which a fatty acid is reacted with a metal oxide or hydroxide, or a metathesis method in which a fatty acid and sodium hydroxide are subjected to a saponification reaction and metathesized with an aqueous metal salt solution.
[0030]
Since metal soap can be produced in a fine powder under low-temperature reaction conditions, the metathesis method is generally adopted. However, in the metathesis method, a large amount of by-product sodium chloride and raw materials are used. The sodium hydroxide used may be mixed with compounds containing nitrogen, phosphorus, sulfur, and chlorine as impurities. For example, inorganic salts composed of potassium ions, calcium ions, sulfate ions, phosphate ions, nitrate ions, etc. may be mixed, and these impurities, especially water-soluble salts, remain even after purification in the final step. There is.
[0031]
The synthetic fiber treatment agent used in the present invention preferably contains substantially no impurities containing metals other than the metal species contained in the metal soap.
[0032]
When magnesium stearate is used as the metal soap, it is preferable that at least one of sodium sulfate and sodium chloride is not substantially contained as an impurity.
[0033]
The average particle diameter of the solid material such as metal soap used in the present invention is preferably 0.1 to 1.0 μm from the viewpoint of improving the handleability and dispersibility.
[0034]
The method for producing the treatment agent for synthetic fibers used in the present invention is not particularly limited, and for example, a predetermined ratio of a solid metal soap such as magnesium stearate as a solid and a smoothing agent such as silicone oil as a liquid. And a method of dispersing the metal soap by wet pulverization. Here, as a pulverizer used for wet pulverization, various wet pulverizers such as a vertical bead mill, a horizontal bead mill, a sand grinder, and a colloid mill can be used.
[0035]
The polyurethane elastic fiber of the present invention refers to a fiber obtained by spinning a polyurethane polymer.
[0036]
The polyurethane polymer in the present invention may be a polyurethane-urea copolymer, or a mixture or copolymer of polyurethane and polyurethane-urea.
[0037]
More specifically, the polyurethane polymer in the present invention comprises two types of segments: (a) a long-chain polyether, a soft segment that is a polyester segment, and (b) an organic isocyanate and a diamine chain extender or diol chain. It contains a hard segment that is a relatively short chain segment derived by reaction with an extender.
[0038]
Typically such polyurethane polymers may be obtained by a prepolymer process in which the prepolymer product obtained by capping a hydroxyl-terminated soft segment precursor with an organic diisocyanate is chain extended with a diamine or diol, and all You may obtain by the one-shot method which puts a raw material in the same bath, and superpose | polymerizes, and may obtain it by another method.
[0039]
Typical polyether soft segments include those derived from polytetramethylene ether glycol (hereinafter abbreviated as PTMG), 3-methyl-1,5-pentanediol, tetrahydrofuran, 3-methyltetrahydrofuran, and the like. Copolymers can be included. Of these, polyethers derived from polytetramethylene ether glycol are preferred. Typical polyester soft segments include (a) ethylene glycol, polytetramethylene ether glycol, 2,2-dimethyl-1,3-propanediol, and (b) dibasic acids such as adipic acid and succinic acid. And the like may be included.
[0040]
The soft segments were formed from typical polyethers and polyesters or from polycarbonate diols such as poly- (pentane-1,5-carbonate) diol and poly- (hexane-1,6-carbonate) diol. A copolymer such as a polyether ester may be used.
[0041]
Typical examples of the organic diisocyanate used in the present invention are bis- (p-isocyanatophenyl) -methane (hereinafter abbreviated as MDI), tolylene diisocyanate (hereinafter abbreviated as TDI), bis- (4-isocyanatocyclohexyl)- Methane (hereinafter abbreviated as PICM), hexamethylene diisocyanate, 3,3,5-trimethyl-5-methylenecyclohexyl diisocyanate, and the like. Among these, MDI is particularly preferable.
[0042]
Various diamines such as ethylene diamine, 1,3-cyclohexane diamine, 1,4-cyclohexane diamine and the like are suitable as a chain extender for forming polyurethane urea. A chain terminator can be included in the reaction mixture to help control the final molecular weight of the polyurethaneurea. Usually, the chain terminator is preferably a monofunctional compound having active hydrogen, for example, diethylamine.
[0043]
The chain extender is not limited to the above amine, and a diol may be used. For example, ethylene glycol, 1,3-propanediol, 4-butanediol, neopentyl glycol, 1,2-propylene glycol, 1,4-cyclohexanedimethanol, 1,4-cyclohexanediol, 1,4- Bis (β-hydroxyethoxy) benzene, bis (β-hydroxyethyl) terephthalate, paraxylylene diol, and the like. The diol chain extender is not limited to only one type of diol, and may be composed of a plurality of types of diols. Moreover, you may use together with the compound containing one hydroxyl group which reacts with an isocyanate group. In this case, various methods such as a melt polymerization method and a solution polymerization method can be adopted as a method for obtaining such a polyurethane. The polymerization formulation is not particularly limited, and examples thereof include a method of synthesizing polyurethane by simultaneously reacting a polyol, a diisocyanate cake, and a chain extender composed of a diol. Good.
[0044]
In the present invention, the polyurethane polymer is an ultraviolet absorber such as benzotriazole, a weathering agent such as a hindered amine, an antioxidant such as a hindered phenol, various pigments such as titanium oxide and iron oxide, barium sulfate, and zinc oxide. In addition, a functional additive containing cesium oxide, silver ions, or the like may be contained.
[0045]
In the present invention, the polyurethane polymer is preferably used as a polyurethane solution using a solvent, preferably used as a polyurethane dispersion using a dispersion medium, and further preferably a mixture thereof.
[0046]
In the present invention, these solutions, dispersions, and mixtures thereof are collectively referred to as stock solutions. In the present invention, a solvent, a dispersion medium, and a mixture thereof are collectively referred to as a medium.
[0047]
Any medium such as a solvent or dispersion medium used for dissolving or dispersing the polyurethane polymer may be used as long as it is inert to polyurethane. , N-dimethylacetamide (hereinafter abbreviated as DMAc), dimethylformamide, dimethylsulfoxide, vinylpyrrolidone and the like are preferably used.
[0048]
The concentration of the stock solution is not particularly limited, but is usually preferably in the range of 25% by weight to 80% by weight.
[0049]
More preferably, it is the range of 30 weight% or more and 60 weight% or less, More preferably, it is the range of 35 weight% or more and 55 weight% or less.
[0050]
If it is less than 25% by weight, the amount of heat required for evaporation of the solvent and the like tends to increase during dry spinning, which tends to make spinning difficult.
[0051]
On the other hand, if it exceeds 80% by weight, the stability of the stock solution is deteriorated. As a result, the spinnability is deteriorated, and the yarn quality tends to be lowered when the degree of polymerization of the polymer is lowered in order to improve the stability of the stock solution.
[0052]
The viscosity of the stock solution is preferably 2500 poise or more and 5500 poise or less. If there is a viscosity of 2500 poise or more, there is little yarn breakage due to a decrease in viscosity when dry spinning, the spinning property is good, and if the viscosity is 5500 poise or less, the pressure loss at the base part can be suppressed to some extent. The yarn quality can be improved.
[0053]
In addition, the value of a viscosity is based on the steel ball drop type viscosity measuring method in 40 degreeC.
[0054]
The polyurethane elastic fiber of the present invention can be obtained by spinning a stock solution. As a spinning method that can be adopted, any method such as a dry spinning method, a melt spinning method, and a wet spinning method may be used.
[0055]
In the present invention, the dry spinning method can be particularly preferably employed. The spinning conditions such as the temperature of the stock solution during dry spinning, the atmospheric temperature, the discharge speed, the die shape, and the yarn take-up speed can be appropriately selected. The number of holes in the die is preferably 1 or more in order to form one or more single yarns.
[0056]
In addition, the fineness, the number of filaments, etc. of the polyurethane elastic fiber of the present invention can be appropriately determined according to the application.
[0057]
Moreover, it is preferable that the treatment agent is applied to the polyurethane elastic fiber mainly in a manufacturing process such as spinning.
[0058]
As the application method, a roller method, a nozzle method, a spray method, or the like can be selected.
[0059]
【Example】
EXAMPLES Hereinafter, although an Example demonstrates this invention further in detail, this invention is not limited to this. The part in an Example and a comparative example represents a weight part, and% represents weight%.
[0060]
In addition, the evaluation method of each characteristic in an Example is demonstrated first.
[0061]
[Dispersion stability and average particle size of polyurethane-based elastic fiber treatment agent]
Regarding dispersion stability, 100 ml of the treatment agent was put into a 100 ml graduated cylinder made of glass with a tight stopper, left at 40 ° C. for 1 week and 1 month, and the appearance of the treatment agent after 1 week and 1 month was observed. Evaluation based on the criteria.
(Double-circle): There was no change in the external appearance in the uniform dispersion state.
A: A transparent layer of less than 5 ml was generated.
Δ: A transparent layer of 5 ml or more was generated.
X: Precipitation occurred.
[0062]
With respect to the average particle size, the treatment agent was diluted so that the metal soap had a concentration of 1000 ppm to prepare a sample. The area-based average particle diameter of this sample was measured at 25 ° C. using an ultracentrifugal automatic particle size distribution analyzer (CAPA-700 manufactured by Horiba, Ltd.).
[0063]
[Applying treatment agent to polyurethane-based elastic fiber]
First, an N, N′-dimethylacetamide (hereinafter abbreviated as DMAC) solution (35% by weight) of polyurethane composed of tetramethylene ether glycol having a molecular weight of 2900, bis- (p-isocyanatophenyl) -methane and ethylene glycol is used. Polymerization was performed to obtain a polymer solution (A).
[0064]
Next, a polyurethane-based dyeing agent DMAC solution (35% by weight) (B) produced by the reaction of t-butyldiethanolamine and methylene-bis- (4-cyclohexylisocyanate) disclosed in US Pat. No. 3,555,115 (B) And an antioxidant DMAC solution (35% by weight) (C), which is a 2 to 1 weight ratio mixture of the condensation polymer of p-cresol and divinylbenzene disclosed in US Pat. No. 3,553,290. Each of A, B, and C was uniformly mixed at 94% by weight, 4% by weight, and 2% by weight to obtain a spinning solution. Using the spinning solution obtained here, dry spinning was performed at a speed ratio of 540 m / min with a speed ratio of godet roller and winder of 1.4, and before the winding, the polyurethane elastic fiber treatment agent was neated by the oiling roller. A traverse that feeds a 20 dtex, monofilament polyurethane-based elastic fiber with a treatment agent attached in an amount of 4.0% by weight to a fiber and gives a winding width of 38 mm to a 58 mm long cylindrical paper tube. It was wound up using a surface drive winder through a guide to obtain 300 g of a wound body. The amount of treatment agent applied was measured according to JIS-L1013 (chemical fiber filament yarn test method) using n-hexane as an extraction solvent.
[0065]
[Evaluation of polyurethane elastic fiber]
The breaking strength and breaking elongation were obtained by subjecting the fiber to a tensile test using an Instron 4502 type tensile tester. These are defined by:
[0066]
300% elongation of a 5 cm (L1) sample was repeated 5 times at a tensile speed of 50 cm / min. The stress at this time was defined as (G1). The length was then held for 30 seconds. Furthermore, it extended | stretched until the fiber cut | disconnected 6th time. The stress at the time of rupture was defined as (G3), and the sample length at the time of rupture was defined as (L3).
[0067]
Hereinafter, the above characteristics are given by the following equation.
[0068]
Strength = (G3)
Elongation = 100 × {(L3) − (L1)) / (L1)}
The unraveling tension was measured using the method described in US Pat. No. 4,296,174, column 4, lines 20 to 45 and FIG. The yarn was peeled off from the side surface of the wound body at 45.7 m / min, and the average tension during peeling of 183 m was measured. The measurement temperature was 25 ° C. and 60% RH. The position of the wound thread body to be measured was the wound body surface layer, the center layer, and the innermost layer. Specifically, the wound body surface layer was a layer obtained by removing about 5 grams of yarn from the surface of the wound body. This is because the winding pattern on the surface of the wound body may be intentionally changed. The innermost layer is a layer that leaves about 5 g of wound yarn on the wound body. The center layer was the intermediate layer between the wound body surface layer and the innermost layer. As the wound body for measuring the unwinding tension, one stored at about 20 ° C. for 3 months or more was used.
[0069]
[Evaluation of scum]
Regarding the scum generation amount, the evaluation at the time of winding and winding the polyurethane-based elastic fiber was evaluated as scum evaluation 1, and the evaluation at the time of using the wound wound body was evaluated as scum evaluation 2.
[0070]
The evaluation at the time of spinning winding was performed by visual observation at the time when the scum was removed from the surface drive roll of the spinning winder and the accumulated state was wound up by 45,000 km, and evaluated according to the following criteria.
A: Almost no scum adhered.
○: Scum slightly adhered, but there was no problem in stable running of the yarn.
X: There was much adhesion and accumulation | storage of scum, and there existed a big problem in the stable driving | running | working of the thread | yarn.
[0071]
When the wound wound body was used, 10 wound bodies were prepared on a miniature warping machine, and wound at 1500 km at a yarn speed of 300 m / min in an atmosphere of 25 ° C. × 65% RH. At this time, the dropout and accumulation state of the scum with respect to the comb guide of the miniature warping machine was visually observed and evaluated according to the following criteria.
A: Almost no scum adhered.
○: Scum slightly adhered, but there was no problem in stable running of the yarn.
X: There was much adhesion and accumulation | storage of scum, and there existed a big problem in the stable driving | running | working of the thread | yarn.
[0072]
[Example 1]
As a dispersion medium, the viscosity at 25 ° C. is 20 × 10 ^-6 m ² A silicone mixture was obtained by mixing 94.3 parts by weight of silicone oil as / S and 0.7 parts by weight of amino-modified silicone as a dispersant (S-1). Next, stearic acid and magnesium oxide are used as raw materials for the metal soap, and 4.0 parts by weight of magnesium distearate (M-1) produced by a dry direct method and containing 30 ppm of sodium is added at 20 to 35 ° C. After mixing until uniform, wet milling was performed using a horizontal bead mill to obtain a synthetic fiber treating agent (T-1) comprising a dispersion in which magnesium distearate (M-1) was colloidally dispersed. . By elemental analysis, 3 ppm of sodium and sulfur were detected in the treating agent (T-1), and the main impurity was sodium sulfate, and it was found that the impurity was not substantially contained.
[0073]
Table 1 shows the composition and evaluation of the treating agent (T-1), and Table 2 shows the evaluation of the polyurethane-based elastic fiber to which (T-1) is imparted.
[0074]
The unraveling tension was slightly lower than that of Comparative Example 1 using the treatment agent (U-1) containing impurities, which was a good result.
[0075]
As a result of scum evaluation 1, it was found that there was almost no scum adhesion.
[0076]
On the other hand, in Comparative Example 1 using the treatment agent (U-1) containing impurities, there is much adhesion and accumulation of scum, and there is a big problem in stable running of the yarn, and cleaning is performed to perform continuous spinning. There was a need.
[0077]
As a result of scum evaluation 2, it was found that there was almost no scum adhesion.
[0078]
On the other hand, Comparative Example 1 using the treatment agent (U-1) containing impurities had a large problem in stable running of the yarn because much scum adhered and accumulated.
[0079]
[Example 2]
To the silicone mixture (S-1) used in Example 1, 6.0 parts by weight of the metal soap (M-1) used in Example 1 which is 1.5 times the amount used in Example 1 was added. Treatment agent (T-2) comprising a dispersion in which magnesium distearate (M-1) is dispersed in a colloidal form by wet grinding using a horizontal bead mill. Got.
[0080]
By elemental analysis, 4 ppm of sodium, sulfur and chlorine were detected in the treating agent (T-2), and it was found that the main impurity was sodium sulfate and contained substantially no impurities.
[0081]
Table 1 shows the composition and evaluation of the treating agent (T-2), and Table 2 shows the evaluation of the polyurethane-based elastic fiber to which (T-2) is imparted.
[0082]
The unraveling tension was slightly lower than that of Comparative Example 2 using the treatment agent (U-2) containing impurities, which was a good result.
[0083]
As a result of scum evaluation 1, it was found that there was almost no scum adhesion.
[0084]
On the other hand, Comparative Example 2 using the treatment agent (U-2) containing an impurity has much adhesion and accumulation of scum and has a large problem in stable running of the yarn, and cleaning is performed to perform continuous spinning. There was a need.
[0085]
As a result of scum evaluation 2, it was found that there was almost no scum adhesion.
[0086]
On the other hand, in Comparative Example 2 using the treatment agent (U-2) containing impurities, there was much adhesion and accumulation of scum, and there was a big problem in stable running of the yarn.
[0087]
[Example 3]
Through the process of refining by-product water-soluble salt using a large amount of washing warm water by the metathesis precipitation method using stearic acid and sodium hydroxide as raw materials for the silicone mixture (S-1) used in Example 1 4.0 parts by weight of magnesium distearate (M-2) having a sodium content of 28 ppm is added and mixed at 20 to 35 ° C. until uniform, and then wet pulverized using a horizontal bead mill and distearic acid. A treating agent (T-3) comprising a dispersion liquid in which a magnesium salt (M-2) was colloidally dispersed was obtained. As a result of conducting elemental analysis to measure the impurity of (T-3), it was found that 28 ppm of sodium, sulfur and chlorine were detected, the main impurity was sodium sulfate, and it was substantially free of impurities.
[0088]
Table 1 shows the composition and evaluation of the treating agent (T-3), and Table 2 shows the evaluation of the polyurethane-based elastic fiber to which (T-3) was added.
[0089]
The unraveling tension was slightly lower than that of Comparative Example 1 using the treatment agent (U-1) containing impurities, which was a good result.
[0090]
From the results of scum evaluation 1 and scum evaluation 2, it was found that there was almost no scum adhesion.
[0091]
[Example 4]
As a dispersion medium, the viscosity at 25 ° C. is 20 × 10 ^-6 m ² A silicone mixture was obtained by mixing 94.3 parts by weight of silicone oil / S and 0.7 parts by weight of carboxyamide-modified silicone as a dispersant (S-2). Magnesium distearate, a magnesium distearate (M-3) having a sodium content of 70 ppm, prepared by a wet direct method using stearic acid and magnesium hydroxide as raw materials in the silicone mixture (S-2) 4.0 parts by weight of M-3) was added and mixed until uniform at 20 to 35 ° C., and then wet milled using a horizontal bead mill to disperse the magnesium distearate (M-3) in a colloidal form. A treatment agent (T-4) comprising a dispersion was obtained. As a result of conducting elemental analysis to measure T-4 impurities, 6 ppm of sodium and sulfur were detected, and it was found that the main impurity was sodium sulfate and contained substantially no impurities.
[0092]
Table 1 shows the composition and evaluation of the treating agent (T-4), and Table 2 shows the evaluation of the polyurethane-based elastic fiber to which (T-4) is imparted.
[0093]
The unraveling tension was slightly lower than that of Comparative Example 3 using the treatment agent (U-3) containing impurities, which was a good result.
[0094]
As a result of scum evaluation 1, it was found that there was almost no scum adhesion.
[0095]
On the other hand, in Comparative Example 3 using the treatment agent (U-3) containing impurities, there is a large amount of scum adhesion and accumulation, and there is a big problem in the stable running of the yarn. Cleaning is performed to perform continuous spinning. There was a need.
[0096]
Even in the result of scum evaluation 2, there was almost no scum adhesion.
[0097]
On the other hand, Comparative Example 3 using the treatment agent (U-3) containing an impurity had much adhesion and accumulation of scum, and had a big problem in stable running of the yarn.
[0098]
[Comparative Example 1]
As a dispersion medium, the viscosity at 25 ° C. is 20 × 10 ^-6 m ² A silicone mixture obtained by mixing 94.3 parts by weight of silicone oil as / S and 0.7 parts by weight of amino-modified silicone as a dispersant was obtained (S-1). Next, magnesium distearate (N-1) of metathesis precipitation method using stearic acid and sodium hydroxide as raw materials was used as metal soap. The sodium content in (N-1) was 1800 ppm. 4.0 parts by weight of (N-1) is added to the silicone mixture (S-1) and mixed at 20 to 35 ° C. until uniform, and then wet pulverized using a horizontal bead mill to disperse magnesium distearate ( A treating agent (U-1) comprising a dispersion in which N-1) was colloidally dispersed was obtained. As a result of conducting elemental analysis to measure the impurities of U-1, 300 ppm of sodium and sulfur were detected, and it was found that the main impurity was sodium sulfate and contained substantially impurities.
[0099]
Table 1 shows the composition and evaluation of the treating agent (U-1), and Table 2 shows the evaluation of the polyurethane-based elastic fiber to which (U-1) was added.
[0100]
As a result of scum evaluation 1, there was much adhesion and accumulation of scum, and even in the result of scum evaluation 2, there was much adhesion and accumulation of scum, and there was a big problem in the stable running of the yarn. The main component of the accumulation was sodium sulfate decahydrate.
[0101]
[Comparative Example 2]
6.0 parts by weight of magnesium distearate (N-1) is added to the silicone mixture (S-1) and mixed at 20 to 35 ° C. until uniform, and then wet pulverized using a horizontal bead mill and distearic acid. A treating agent (U-2) comprising a dispersion in which the magnesium salt (N-1) was dispersed in a colloidal form was obtained. As a result of conducting elemental analysis to measure U-2 impurities, 470 ppm of sodium, sulfur and chlorine were detected, and it was found that the main impurity was sodium sulfate and contained substantially impurities. Table 1 shows the composition and evaluation of the treatment agent (U-2), and Table 2 shows the evaluation of the polyurethane-based elastic fiber to which (U-2) was added.
[0102]
As a result of scum evaluation 1, there was much adhesion and accumulation of scum, and even in the result of scum evaluation 2, there was much adhesion and accumulation of scum, and there was a big problem in the stable running of the yarn. The main components of the accumulation were sodium sulfate decahydrate and sodium chloride.
[0103]
[Comparative Example 3]
For the silicone mixture (S-2), magnesium distearate (N-2) of metathesis precipitation method using stearic acid and sodium hydroxide as raw materials was used as metal soap. Add 4.0 parts by weight of (N-2) to silicone mixture (S-2) whose sodium content of (N-2) was 2200 ppm by elemental analysis, and mix until uniform at 20-35 ° C. After that, wet milling was performed using a horizontal bead mill to obtain a treatment agent (U-3) comprising a dispersion in which magnesium distearate (N-2) was dispersed in a colloidal form. As a result of conducting elemental analysis for measuring the impurities of U-1, it was found that 330 ppm of sodium and sulfur were detected, the main impurity was sodium sulfate, and the impurities were substantially contained.
[0104]
Table 1 shows the composition and evaluation of the treating agent (U-3), and Table 2 shows the evaluation of the polyurethane-based elastic fiber to which (U-3) was added.
[0105]
As a result of scum evaluation 1, there was much adhesion and accumulation of scum, and even in the result of scum evaluation 2, there was much adhesion and accumulation of scum, and there was a big problem in the stable running of the yarn. The main component of the accumulation was sodium sulfate decahydrate.
[0106]
[Table 1]

[0107]
[Table 2]

[0108]
【The invention's effect】
The polyurethane-based elastic fiber of the present invention described above can be stably operated to prevent scum from dropping off and accumulating on guides when used in a post-processing step, and has excellent knitted and woven fabric quality. There is an effect that can be done.

Claims (7)

A metal soap is contained and a treatment agent having an impurity of 50 ppm or less is provided, and the impurity is an inorganic salt containing at least one of nitrogen, phosphorus, sulfur, and chlorine. Polyurethane elastic fiber. The polyurethane elastic fiber according to claim 1, wherein the metal soap is a fatty acid metal salt. The polyurethane-based elastic fiber according to claim 2, wherein the fatty acid metal salt is magnesium stearate. The polyurethane-based elastic fiber according to any one of claims 1 to 3, wherein the impurity contains a metal other than the metal species contained in the metal soap. The polyurethane elastic fiber according to any one of claims 1 to 4 , wherein the impurity is a water-soluble metal salt. The polyurethane elastic fiber according to any one of claims 1 to 5 , wherein the impurity is sodium sulfate and / or sodium chloride. A polyurethane system characterized by containing a metal soap and providing a treating agent having an impurity of 50 ppm or less, and wherein the impurity is an inorganic salt containing at least one of nitrogen, phosphorus, sulfur and chlorine A method for producing elastic fibers.