JP2700299B2 - Spinning oil for synthetic fibers - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a spinning oil agent for synthetic fibers. More particularly, it relates to a spinning oil agent suitable for high-speed spinning.

[0002]

2. Description of the Related Art Conventionally, in a synthetic fiber spinning process, an aqueous emulsion of an oil agent comprising a mixture of a lubricant and a surfactant is supplied. The conventional oil agent does not uniformly adhere to the fiber yarn in a high-speed spinning process that has been industrialized in recent years, and the scattering of the emulsion causes problems such as loss of the oil agent and contamination of the working environment.

[0003] In order to solve this problem, it has been proposed to include perfluoroalkylamine oxide, polyoxyethylene octyl ether, and the like in an oil agent (JP-A-2-47361 and JP-A-3-977961).

[0004]

However, when the spinning speed is 3
As a spinning oil for a high-speed spinning process (high-speed spin draw, draw spin, etc.) of 000 m / min or more, a high-performance oil having further improved adhesion and anti-scattering properties is required.

[0005]

Means for Solving the Problems The present inventors have conducted intensive studies to obtain an oil agent having improved adhesion and scattering prevention, and as a result, have found that an oil agent having a specific composition is dramatically effective. The present invention has been reached.

That is, the present invention provides a fatty acid ester (1)
Salt (2) of an organic phosphate ester anion (a) having an alkyl group having 6 to 14 carbon atoms and a quaternary ammonium cation (b) having an alkyl group having 6 to 14 carbon atoms, and other surfactants A spinning oil agent for synthetic fibers, which comprises (3) and the content of the fatty acid ester (1) is 50 to 90% by weight based on the total weight of the oil agent.

[0007] The fatty acid ester (1) in the present invention comprises:
Monoesters of natural or synthetic monohydric alcohols and monohydric carboxylic acids (eg, isopropyl myristylate, butyl stearate, isooctyl palmitate,
Esters of isooctyl stearate, isotridecyl stearate, isotridecyl oleate, isostearyl oleate, etc .; monohydric carboxylic acids with dihydric or higher alcohols (eg, neopentyl glycol dilaurate, neopentyl glycol di) Oleate, trimethylolpropane trilaurate, glycerin monooleate, glycerindiolate, glycerin trioleate, pentaerythritol tetraoleate, sorbitan tetraoleate, sorbitol hexaoleate, etc.); divalent or higher carboxylic acids and monovalent Esters with alcohols (dioctyl sebacate, dioleyl adipate, dilauryl phthalate, diisotridecylthiodipropionate, etc.); alkylenes of alcohols or alkylphenols Ester of oxide adduct and carboxylic acid (for example, ester of ethylene oxide 2 mol adduct of isotridecyl alcohol (hereinafter abbreviated as EO2) and thiodipropionic acid, propylene oxide of bisphenol A (hereinafter abbreviated as PO) EO addition And lauric acid, and an ester of trimethylolpropane PO adduct with coconut fatty acid.

Preferred among these are and.

The organic phosphate anion (a) having an alkyl group having 6 to 14 carbon atoms in the present invention includes n
-Octyl phosphate, 2-ethylhexyl phosphate, n-octyl EO2 phosphate, dovanol 2
3 (Mixed alcohol having a side chain ratio of about 20%, manufactured by Mitsubishi Yuka Co., Ltd. and having 12 or 13 carbon atoms). Anions such as phosphate, tetradecyl phosphate and dodecyl phosphate.

Among these, anions such as n-octyl phosphate and 2-ethylhexyl phosphate are particularly preferred.

The quaternary ammonium cation (b) having an alkyl group having 6 to 14 carbon atoms in the present invention includes:
Examples include quaternary ammonium cations such as trimethyloctyl ammonium, tributyl octyl ammonium, trimethyl coconut alkyl ammonium, trimethyl hexyl ammonium, trimethyl decyl ammonium, trimethyl tetradecyl ammonium, and monomethyl trioctyl ammonium.

[0012]

The organic phosphate ester anion (a) having an alkyl group having 6 to 14 carbon atoms according to the present invention,
The salt (2) with the quaternary ammonium cation (b) having an alkyl group of from 14 to 14 may be separately added to the base oil and then converted into a salt, or may be previously mixed as a salt.

The organic phosphate ester anion (a) having an alkyl group having 6 to 14 carbon atoms according to the present invention and the anion (a) having 6 to 14 carbon atoms.
The salt (2) with the quaternary ammonium cation (b) having an alkyl group of 14 can be produced by the following method or the like. For example, in the case of a salt of octyl phosphate and trimethyloctyl ammonium, 3 moles of octyl alcohol and 1 mole of phosphoric anhydride are reacted at 60 to 70 ° C. to obtain mono-, di-, and mixed esters of octyl phosphate. Separately, 1 mol of dimethyloctylamine and equimolar amounts or more of dimethyl carbonate and methanol are charged into an autoclave, and about 120 kg under a pressure of about 5 kg / cm ^2.
By reacting at a temperature of ° C, a methanol solution of trimethyloctyl ammonium methyl carbonate is obtained. Next, a methanol solution of trimethyloctyl ammonium methyl carbonate is gradually added to the mono-, di-, and mixed esters of octyl phosphoric acid at 80 to 90 ° C, and the generated carbon dioxide and methanol are distilled off. Next, water was added, and after sufficiently performing an anion exchange reaction, the mixture was further diluted with water.
An aqueous solution of trimethyloctyl ammonium octyl phosphate is obtained.

Other surfactants (3) in the present invention
Examples include nonionic surfactants and ionic surfactants.

As the nonionic surfactant, one having 1 carbon atom
EO adducts of 0 to 18 monohydric alcohols (eg, lauryl alcohol EO adduct, isotridecyl alcohol EO adduct and isostearyl alcohol EO adduct); higher fatty acid esters of polyethylene glycol [eg, polyethylene glycol ( Number average molecular weight 20
0) Monolaurate and polyethylene glycol (number average molecular weight 300) mono-tallow fatty acid ester]; EO adduct of hydrogenated castor oil; EO adduct of alkylamine; higher fatty acid alkanolamide and the like.

Among them, those having 10 to 1 carbon atoms are preferred.
EO adducts of 8 monohydric alcohols, particularly preferably low mol (7 mol or less) adducts of EO having 10 to 18 carbon atoms.

Examples of the ionic surfactant include anionic surfactants (for example, alkali metal salts of alkyl sulfonates, alkali metal salts or amine salts of higher aliphatic carboxylic acids, alkali metal salts or amine salts of alkyl phosphates, polyoxyalkylene alkyls). Phosphate alkali metal salts and sulfates of animal and vegetable oils); amphoteric surfactants (betaine type and amino acid type); cationic surfactants (amine salt type and quaternary ammonium salt type); dimethylsiloxane group or perfluoroalkyl group And an ionic surfactant having the formula:

Of these, anionic surfactants are preferred, and a combination of two or more of the above is effective.

The oil agent of the present invention may further contain polyhydric alcohols and / or oxycarboxylic acids. Polyhydric alcohols include polyhydric alcohols and derivatives thereof (ether-containing polyols). For example, ethylene glycol, propylene glycol, diethylene glycol, trimethylolpropane,
Glycerin, diglycerin, decaglycerin and glycerin monomethyl ether are included. Preferred among these are glycerin and decaglycerin.

The oxycarboxylic acids include oxycarboxylic acids and neutralized salts thereof. Examples of oxycarboxylic acids include, for example, glycolic acid, lactic acid, malic acid,
Tartaric acid and citric acid are mentioned. Examples of neutralizing salts of oxycarboxylic acids include alkali metal salts (eg, Na salt and K salt); ammonium salts (eg, tetramethyl ammonium salt, monomethyl triethyl ammonium salt, monomethyl triisopropyl ammonium salt, trimethyl octyl ammonium salt); organic Amine salts (eg, monoethanolamine salt, diethanolamine salt, dibutylethanolamine salt, triethanolamine salt, triethylamine salt, tributylamine salt and octylamine salt). Among these, lactic acid and / or an organic amine salt of lactic acid are preferred.

In the present invention, the surface tension of a 10% by weight aqueous emulsion at 25 ° C. is 26 to 30 dynes / c.
m is preferred. Particularly preferred is 27-29 dynes / c
m. If it is less than 26 dynes / cm, the dripping of the emulsion tends to increase. On the other hand, 30 dynes / cm
When it exceeds, the dispersion of the emulsion tends to increase.

Further, 2% of a 10% by weight aqueous emulsion
The contact angle with the polyester film at 5 ° C.
Those having an angle of 30 ° or less after 1 second of contact and 5 ° or less after 60 seconds of contact are preferable because the dispersion of the emulsion is extremely small.

In the present invention, the content of the fatty acid ester is usually 50 to 90% by weight, preferably 55 to 85% by weight, based on the total weight of the oil agent. When the content of the fatty acid ester is less than 50% by weight, the smoothness tends to decrease.
If it exceeds 90% by weight, the stability of the emulsion tends to decrease.

In the present invention, a salt of an organic phosphate ester anion (a) having an alkyl group having 6 to 14 carbon atoms and a quaternary ammonium cation (b) having an alkyl group having 6 to 14 carbon atoms (2) Content is based on the total weight of the oil
Usually, it is 0.5 to 8% by weight, preferably 1 to 6% by weight. If the content is less than 0.5% by weight, it tends to be difficult to obtain the emulsion characteristics of the present invention. If it exceeds 8% by weight, the smoothness tends to decrease.

In the present invention, the content of the nonionic surfactant is usually 5 to 25% by weight, preferably 10 to 20% by weight, based on the total weight of the oil agent. If the content is less than 5% by weight, the stability of the emulsion tends to decrease. 25
If the content exceeds% by weight, the smoothness tends to decrease and the sizing characteristics tend to be inferior.

In the present invention, the content of the ionic surfactant is usually 3 to 10, preferably 4 to 8% by weight based on the total weight of the oil agent. If the content is less than 3% by weight, it tends to be difficult to obtain the emulsion characteristics of the present invention.
Also, the antistatic performance is reduced. If the content exceeds 10% by weight, the smoothness tends to decrease, and the amount of the oil agent dropped onto the rollers and guides tends to increase.

In the present invention, the content of the polyhydric alcohol is usually 7% by weight or less, preferably 5% by weight or less based on the total weight of the oil agent. If it exceeds 7% by weight, the stability of the stock oil solution tends to decrease.

In the present invention, the content of the oxycarboxylic acid is usually 8% by weight or less, preferably 6% by weight or less based on the total weight of the oil agent. If it exceeds 8% by weight, the stability of the stock oil solution and the stability of the emulsion tend to decrease.

Any component can be used in the oil agent of the present invention as long as it does not deviate from the emulsion characteristics of the present invention.
Optional ingredients include lubricants (eg, mineral oils, silicone oils, and polyethers), oiliness improvers (eg, higher fatty acids and higher aliphatic amines), extreme pressure additives, rust inhibitors, antioxidants, and Other functional additives and the like can be contained, and these types are not particularly limited.

The oil agent of the present invention is supplied to the spun yarn as an aqueous emulsion in the step of melt-spinning synthetic fibers.

The concentration of the emulsion is 0.5 to 30% by weight.
It is possible to select an arbitrary concentration within the range. Preferably 5
-20% by weight.

The method of lubricating the emulsion is not particularly limited, and any method such as nozzle lubrication and roller lubrication may be used.

[0034] The amount of the oil agent to be attached is 0.3% in terms of the pure content with respect to the fiber.
To 2.0% by weight, preferably 0.5 to 1.5% by weight.

The synthetic fibers to be applied include polyester, nylon, polypropylene and the like. There is no particular limitation on the yarn brand, but the yarn brand is suitable for a yarn for knitting and weaving of 200 denier or less.

[0036]

EXAMPLES The present invention will be further described with reference to examples and the like, but the present invention is not limited to these examples. In the following, parts and% indicate parts by weight and% by weight, respectively.

Example 1, Comparative Examples 1 to 4 The compounds shown in Table 2 were added to the base oils shown in Table 1 and
(Example 1 and Comparative Examples 1 to 4) An oil having the composition described was prepared, and a 10% aqueous emulsion of the oil was prepared. Next, a commercially available polyester filament (75 denier, 36
The defatted yarn (filament) is run at a speed of 500 m / min while adjusting the tension to 10 g, and a 10% emulsion of each oil is quantified so as to be 10% of the running yarn weight (target oil adhesion: 1.0%). The pump was adjusted to refuel the nozzle. An interlace nozzle was set at 6 cm immediately below the oil supply nozzle, and compressed air of 0.5 kg / cm 2 was supplied to forcibly disperse the oil agent and then wound up. Table 3 shows the evaluation results of the physical properties and functions of each oil emulsion and the oil adhesion efficiency of the wound yarn.

[Evaluation Items and Methods] Surface tension: The surface tension of a 10% emulsion was measured using CBVP-A manufactured by Kyowa Interface Science Co., Ltd.
It was measured with a type 3 automatic surface tensiometer. (Unit: Dyne / c
m, measurement temperature: 25 ° C.) Contact angle: The contact angle at 1 second and 60 seconds after contact with a 10% emulsion polyester film was measured with a Kyowa Interface Science Co., Ltd. CA-Z type automatic contact angle meter (image processing method). It was measured. (Unit: degree, measurement temperature: 25 ° C) Wettability: 5% of 10% emulsion in 100cc beaker
After collecting 0 cc and adjusting the temperature in a thermostat at 25 ° C. for 15 minutes, the time (sec) until a wool felt of 2 cm × 2 cm × 3 mm (thickness) was gently settled in the floating liquid on the emulsion surface was measured. The average was calculated by performing the measurement five times. (Unit: second) Oil adhesion efficiency: Measure the oil adhesion amount (P%) of the lubricating yarn,
The following formula shows the oil agent adhesion efficiency. Oil agent adhesion efficiency = P x 100 [%]

[0039]

[Table 1]

[0040]

[Table 2]

[0041]

[Table 3]

[0042]

As is clear from the results shown in Table 3, the oil agent of the present invention (Example 1) has high adhesiveness.

Next, in Example 3 of Table 3 and 10 of Comparative Examples 1 to 3,
A 50 denier 36 filament polyester fiber was spun by a spin draw method (drawing speed: 3000 m / min, drawing speed: 5000 m / min, oil supply: nozzle oiling method) using the% emulsion. Table 5 shows the evaluation results of the number of yarn breaks during spinning (per hour), the quality of the raw yarn (the number of fluffs, the dyeability), and the comparison results of emulsion scattering and scum generation. The number of fluff was obtained by measuring the number of fluff of 20 obtained yarn cakes and expressing the number per 1 million meters. For the dyeability, a fabric was prepared from the obtained yarn, and the fabric was dyed to determine the degree of stain spots.

[0045]

[Table 4]

From the results shown in Table 4, it can be seen that the oils of the examples of the present invention showed less emulsion scattering than the conventional oils and reduced the occurrence of scum in the yarn guides (guides and rollers), so that good results were obtained. . In addition, process passability equal to or higher than that of the conventional yarn was exhibited.

[0047]

The spinning oil agent of the present invention exhibits excellent spinning properties during melt spinning and stretching of polyester and nylon. In particular, in a high-speed spinning process (high-speed spin draw, draw spin) for obtaining a filament yarn that can be knitted in one step with a spinning speed of 3000 m / min or more,
The adhesion efficiency of the emulsion is extremely high, and the desired smoothness, antistatic property, anti-metal abrasion property and the like can be imparted to the fiber, and both the spinning property and the post-processability are improved. Further, since the scattering of the emulsion is small, effects such as a reduction in oil agent loss and an improvement in the yarn-making operation environment can be expected. Further, since the occurrence of scum is small, an effect of reducing work such as extension of a cleaning cycle can be expected.

 ──────────────────────────────────────────────────続 き Continuation of the front page Examiner Ruka Fuchino (56) References JP-A-3-97961 (JP, A) JP-A-54-125791 (JP, A) JP-A-62-15382 (JP, A) JP-A-63-288269 (JP, A)

Claims (6)

(57) [Claims] 1. Fatty acid ester (1), having 6 to 14 carbon atoms
Organic phosphate ester anion having an alkyl group (a)
And a salt (2) with a quaternary ammonium cation (b) having an alkyl group having 6 to 14 carbon atoms, and another surfactant (3), and the content of the fatty acid ester (1) is A spinning oil for synthetic fibers, which is 50 to 90% by weight based on the total weight of the oil. 2. The spinning oil agent for synthetic fibers according to claim 1, further comprising a polyhydric alcohol and / or an oxycarboxylic acid. 3. The content of the fatty acid ester (1) is 55 to 85% by weight based on the total weight of the oil agent.
The spinning oil agent for synthetic fibers according to the above. 4. The spinning oil agent for synthetic fibers according to claim 1, wherein the content of the salt (2) of (a) and (b) is 1 to 6% by weight based on the total weight of the oil agent. 5. The spinning oil agent for synthetic fibers according to claim 1, wherein the surface tension of the 10% by weight aqueous emulsion at 25 ° C. is 26 to 30 dynes / cm. 6. The method according to claim 1, wherein the contact angle of the 10% by weight water-based emulsion to the polyester film at 25 ° C. is 30 ° or less after 1 second of contact and 5 ° or less after 60 seconds of contact. The spinning oil agent for synthetic fibers according to any one of the above.