JPH10251967A - False-twisting oil for synthetic fiber - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain the subject false-twisting oil that scarcely occurs tar or scum in and hot type false-twisting processes by adding a polyether lubricant, a fluorine containing acidic phosphoric ester and an organic acid to the yarn false-twisting oil. SOLUTION: This false-twisting oil contains (A) 50-99wt.% of polyether lubricant, (B) 0.01-0.08wt.% of a fluorine-containing acidic phosphoric ester and (G) 0.1-3.0wt.% of an organic acid as maleic acid. This oil is applied to the yarn immediately after being extruded from the spinneret in the form of an aqueous solution or emulsion and is suitable for production of DTY(draw- textured yarn) or of POY(partially oriented yarn).

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a spinning oil agent for synthetic fibers. More specifically, the present invention relates to a spinning oil agent suitable for thermoplastic synthetic fibers subjected to false twisting.

[0002]

2. Description of the Related Art Conventionally, as a spinning oil agent for false twisted yarn, an oil agent based on a polyether-based lubricant has been used for the purpose of minimizing the generation of tar on a hot plate.
With the recent increase in processing speed, an oil agent with less and more tar has been desired. On the other hand, in order to prevent polyester oligomers and polymer debris from dropping onto the hot plate and being thermally degraded, oils containing a small amount of polyalkylene oxide-modified polysiloxane (such as JP-B-63-57548) or specific heat Method of attaching and treating an oil agent containing a perfluoro group-containing compound exhibiting decomposition behavior (Japanese Patent Publication No. Sho 62)
-44072). But the former,
In high-speed false twisting with a radiant heat high temperature heater that has recently been put into practical use, the heater temperature becomes 500 ° C or higher, and silica sticks to the guide in the heater due to thermal decomposition, causing fluff and yarn breakage. Has been pointed out. The latter is effective only when the perfluoroalkyl group-containing compound dropped onto the hot plate at a specific temperature is thermally decomposed, and is not necessarily sufficient in an actual process.

[0003]

From the above-mentioned current situation, oils which do not generate tar or scum in both types of false twisting processing of a hot plate contact heating type and a non-contact heating type using a radiant heat type high temperature heater are strong. It has been demanded.

[0004]

Means for Solving the Problems The inventors of the present invention have conducted intensive studies for the purpose of solving the above-mentioned problems, and as a result, POY treated with an oil agent containing a specific compound has a hot plate contact heating type false twisting process. In addition, the production of tar was remarkably suppressed, and it was found that almost no scum was generated even in high-speed processing by a radiant heat high temperature heater, and the present invention was reached.

That is, in the present invention, 50 to 99% by weight of a polyether-based lubricant (A), 0.01 to 0.08% by weight of a fluorine-based acidic phosphoric acid ester (B), and 0% by weight of an organic acid (C) are used. It is a spinning oil agent for synthetic fibers, characterized in that it contains 0.1 to 3.0% by weight.

[0006]

DETAILED DESCRIPTION OF THE INVENTION In the present invention, a polyether-based lubricant is a compound obtained by copolymerizing an alcohol having at least one hydroxyl group in a molecule with an alkylene oxide having 2 to 4 carbon atoms and a compound derived therefrom. Is raised.

The alcohol may be any natural or synthetic monohydric alcohol having 1 to 30 carbon atoms (methanol, ethanol, isopropanol, butanol, isoamyl alcohol, 2-ethylhexanol, lauryl alcohol, isotridecyl alcohol, isocetyl alcohol). , Stearyl alcohol, isostearyl alcohol, etc.), dihydric alcohols (ethylene glycol, propylene glycol, neopentyl glycol, hexylene glycol, etc.) and trivalent or higher alcohols (glycerin, trimethylolpropane, pentaerythritol, sorbitan, sorbitol, etc.) ).

The alkylene oxides having 2 to 4 carbon atoms include ethylene oxide (hereinafter abbreviated as EO), 1,2-propylene oxide (hereinafter abbreviated as PO), 1,2-butylene oxide (hereinafter abbreviated as BO), and tetrahydrofuran (hereinafter abbreviated as THF). Abbreviation).

When EO is copolymerized with another alkylene oxide, the proportion of EO is 5 to 80% by weight. The addition mode may be either random addition or block addition.

The weight average molecular weight of the polyether-based lubricant is suitably from 1,000 to 20,000.

As the compound derived from the above-mentioned copolymerized addition compound of alkylene oxide, a compound in which a terminal hydroxyl group is alkoxylated and / or acylated with an alkyl group having 1 to 12 carbon atoms, or a compound having 2 to 12 carbon atoms. Compounds esterified with a dicarboxylic acid and compounds urethanized with an aliphatic or aromatic diisocyanate compound, and the like can be given.

Specific examples of the polyether-based lubricant include:
For example, [butanol (EO / PO) random adduct, E
O / PO = 50/50% by weight, weight average molecular weight = 140
0], [hexylene glycol (EO / PO) random adduct, EO / PO = 40/60% by weight, weight average molecular weight = 4000], [trimethylolpropane (PO)
(EO) Methyl ether of block adduct, EO / PO
= 20/80% by weight, weight average molecular weight = 5000] and the like, but is not limited thereto.

In the present invention, the blending amount of the polyether-based lubricant is 50 to 99% by weight based on the total weight of the oil agent.

In the present invention, the fluorine acid phosphate (B) is at least one compound represented by the following general formula. Rf; 1 or 2 integer p;; alkylene group m of 2 to 4 carbon atoms; perfluoroalkyl group A ¹ in having 4 to 18 carbon atoms integer X 0 or _{1~20: - (CH 2) n} -, - SO ₂ NR ² -A ² -or -CONR ³ -A ² -n: 0 or an integer of 1 to 4 A ² : alkylene group having 1 to 8 carbon atoms R ¹ , R ² ; H or 1 to 8 carbon atoms Alkyl group

In the present invention, the fluorine content in the fluorine acid phosphate (B) is usually from 5 to 90% by weight. Specific examples of (B) include the following compounds. Compound _{B-1 [C 8 F 17} SO 2 N (C 3 H 7) C 2 H 4 O] P = O (OH) 2 Compound _{B-2 [C 8 H 17} C 2 H 4 O] 2 P = O (OH) a compound _{B-3 [C 8 H 17} C 2 H 4 (OC 2 H 4) 10 O] 2 -P = O (OH) number of carbon atoms in the preferred are Rf among these 6-12 , M = 1. Also particularly preferably, X;
-SO ₂ NR ² -A ^2- , where p = 0.

In the present invention, the content of the fluoroacid phosphate (B) is 0.01 to 0.01% based on the total weight of the oil agent.
0.08% by weight, preferably 0.02 to 0.06%
% By weight. If the content is less than 0.01% by weight, the effect of preventing tar on a hot plate is reduced. If the content is more than 0.08% by weight, slightly generated tar tends to be difficult to wash with water.

Organic acids (C) used in the present invention
Is an aliphatic monocarboxylic acid having 8 to 18 carbon atoms (caprylic acid, lauric acid, oleic acid, or the like), and having 4 to 40 carbon atoms.
Aliphatic dicarboxylic acids (maleic acid, adipic acid, dodecenylsuccinic acid, pentadecenylsuccinic acid, dimer acid, etc.), aromatic carboxylic acids (benzoic acid, salicylic acid, phthalic acid, etc.), aliphatics having 8 to 18 carbon atoms Acidic phosphates of alcohols, acidic phosphates of compounds obtained by adding EO and / or PO to aliphatic alcohols having 8 to 18 carbon atoms, and EO to alkylphenols having 8 to 18 carbon atoms
And / or an acidic phosphoric acid ester of a compound to which PO is added, and an amine salt and / or a quaternary ammonium salt thereof, wherein the pH of a 1% water diluent is 6 or less. Preferred among these are dicarboxylic acids and their quaternary ammonium salts.

In the present invention, the content of the organic acids is 0.1 to 3.0% by weight, particularly preferably 0.3 to 1.5% by weight, based on the total weight of the oil agent. When the content of the organic acids is less than 0.1% by weight, the effect of preventing tar on the hot plate decreases. If the content exceeds 3% by weight, the effect of preventing tar is reduced.

Any component can be used in the spinning oil agent for synthetic fibers of the present invention as long as it does not deviate from the object of the present invention. Optional components include lubricants (eg, mineral oil, fatty acid ester oil, etc.), emulsifiers (nonionic activators such as higher alcohol EO adducts and higher fatty acid EO adducts), and antistatic agents (anionic activators, cationic activators). , An amphoteric activator), an extreme pressure additive, a rust inhibitor, an antioxidant, and other functional additives, and the like, and there is no particular limitation on these types.

The spinning oil agent for synthetic fibers of the present invention exhibits a particularly excellent tar-preventing action when the pH of the 10% emulsion is adjusted to 5.0 to 7.0.

The spinning oil agent for synthetic fibers of the present invention is supplied as an aqueous solution or an aqueous emulsion to the yarn immediately after spinning in the step of melt-spinning thermoplastic synthetic fibers.

The concentration of the aqueous solution or aqueous emulsion can be selected from any concentration in the range of 0.5 to 20% by weight. Preferably it is 5.0-15.0% by weight.

The method of oiling the aqueous solution is not particularly limited, and may be any of metering oiling via a nozzle, roller oiling, and a combination thereof.

[0024] The amount of the oil agent attached is 0.1
To 1.5% by weight, preferably 0.2 to 1.0% by weight.

Examples of the synthetic fibers to be applied include polyester, polyamide and polypropylene. Although the yarn brand is not particularly limited, it is suitable for POY (partially oriented yarn) for DTY (drawn false twisted yarn) of 450 denier or less.

[0026]

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.

Examples 1 to 5 and Comparative Examples 1 to 7 Using the following base oils and components, the oils of the present invention and the oils obtained by mixing the comparative oils at the ratios shown in Table 1 were prepared in the following manner. The degree of tar generation on the hot plate, the removability of tar, and the amount of scum generated at 500 ° C. were evaluated. Table 2 shows the results. Base oil: Butanol (EO / PO) random adduct 60 parts (EO / PO = 50/50, average molecular weight: 1400) Lauryl alcohol (PO) (EO) block adduct 20 parts (EO / PO = 40/60, average) Molecular weight: 1400) Propylene glycol (EO / PO) random adduct 10 parts (EO / PO = 50/50, average molecular weight: 8000) Lauric acid EO 10 mol adduct 8 parts 1 part of alkansphonate Na having 14 to 16 carbon atoms phosphate K 1 part compound of isostearyl alcohol EO5 mole adduct _{B-1 [C 8 F 17} SO 2 N (C 3 H 7) C 2 H 4 O] P = O (OH) 2 compound B-2 [C _{8 H 17 C 2 H 4 O} ] 2 P = O (OH) compound _{B-3 [C 8 F 17} C 2 H 4 O (C 2 H 4 O) 10] 2 -P = O (OH) compound C- 1 bird Ethylmethylammonium phthalate Compound C-2 Pentadecenyl succinic acid Compound D-1 Poly (EO, PO) modified dimethylsiloxane Compound D-2 20 mol EO adduct of C ₈ F ₁₇ SO ₂ NC ₂ H ₄ OH Compound D- ₃ C ₈ F ₁₇ SO 3 Na

[0028]

[Table 1]

[Evaluation method] Degree of tar generation on a hot plate: width 3 cm, length 30 cm
Set the SUS plate at an inclination angle of 50 degrees and set the surface temperature to 2
Keep at 20 ° C. At the top of this hot plate, apply 3 ml /
The mixture is dropped at a speed of 1 minute for 3 hours, and the degree of generation of tar on the hot plate is evaluated and determined. Tar removal: 50 mm in diameter, 10 mm in height
Was collected in a SUS petri dish and heated in a circulating drier at 220 ° C. for 10 hours. The residue after heating is wiped with a cloth moistened with water, and the degree of its removal is evaluated. Judgment criteria A: The whole amount is easily removed even if it is wiped lightly. ：: Partially removed when gently wiped, but removed when strongly rubbed. Δ: More than half is not removed when gently wiped. Some parts remain even if rubbed strongly. ×: Not removed even if strongly rubbed. Amount of scum generated at 500 ° C: 50 m in diameter of the oil agent shown in Table 1
0.5 g is collected in a magnetic dish having a height of 10 mm and heated in a circulating drier at 220 ° C. for 10 hours. Then, the mixture was heated in an electric furnace at 500 ° C. for 20 minutes, and the amount of scum generated was evaluated.

[0030]

[Table 2]

From Table 2, it can be seen that the oil agent of the present invention significantly suppresses the generation of tar on a hot plate at 220 ° C .;
It is clear that scum generation under high temperature heating of ℃ is small.

The polyester was melt-spun at a winding speed of 3200 m / min, and a 230 denier / 36 filament P
The OY was wound up. At this time, Example 1 and Comparative Example 1,
The 10% emulsions of the oils of Nos. 5 and 6 were supplied with nozzles so that the net amount of adhesion was 0.3%. These POYs
Was subjected to stretch false twisting at a hot plate temperature of 220 ° C. and at a processing speed of 800 m / min. Table 3 shows the evaluation results of the degree of tar generation on the hot plate and the DTY fluff one month after the start of processing. The DTY fluff was unwound from the DTY obtained one month after the start of operation at an unwinding speed of 150 m / min, and a fluff tester (DT-1 manufactured by Toray Industries, Inc.).
04 type), the number of fluff per 10,000 m length was measured.

[0033]

[Table 3]

The polyester was melt-spun at a winding speed of 2700 m / min, and POY of 270 denier / 36 filaments was wound. At this time, the 10% emulsions of the oils of Example 1 and Comparative Examples 1, 5 and 6 were supplied to the nozzles so that the net amount of adhesion was 0.3%. Using these POYs, a triaxial circumscribed friction system using a urethane disk, a radiant heat type high temperature heater temperature of 500 ° C.,
Stretch false twisting was performed at a processing speed of 1100 m / min. Table 4 shows the results of the evaluation of the degree of scum attached to the guide in the heater and the number of DTY fluffs after three months from the start of processing.

[0035]

[Table 4]

Tables 3 and 4 show that the oil of the present invention has excellent heat resistance in the false twisting process using a hot plate contact heating method and in the false twisting process using a radiant heat high temperature heater.
It is clear that the quality of TY is also excellent.

[0037]

The POY produced with the spinning oil agent for synthetic fibers of the present invention can be used for the conventional twisting by hot plate contact heating and non-contact heating by radiant heat high temperature heater. In any case, high quality DTY
As a result, it is possible to expect effects such that the heater cleaning cycle is greatly extended, and DTY productivity and workability are greatly improved.

 ──────────────────────────────────────────────────続 き Continuing from the front page (72) Inventor Shusuke Sakai 1 at 11-11 Hitotsubashi Nohoncho, Higashiyama-ku, Kyoto Inside Sanyo Chemical Industry Co., Ltd.

Claims (5)

[Claims] 1. A polyether-based lubricant (A) of 50 to 9
9% by weight, 0.01% of a fluoro acid phosphate (B)
To 0.08% by weight, and 0.1 to 0.1% by weight of the organic acids (C).
A spinning oil agent for synthetic fibers, which contains 3.0% by weight. 2. The spinning oil agent for synthetic fibers according to claim 1, wherein the fluoro acid phosphate is a monophosphate having a perfluoroalkyl group having 6 to 12 carbon atoms in the molecule. 3. The spinning oil agent for synthetic fibers according to claim 2, wherein the fluorine acid phosphate has a sulfonamide group in the molecule. 4. The spinning oil agent for synthetic fibers according to claim 1, wherein the pH of the 10% emulsion is from 5.0 to less than 7.0. 5. The spinning oil agent for synthetic fibers according to claim 1, wherein the use is for POY-DTY of polyester or polyamide.