JP2948874B2 - Spinning oil for synthetic fibers - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to a spinning oil agent for synthetic fibers. More specifically, the present invention relates to a spinning oil agent for synthetic fibers that exhibits good spinnability and spinnability when used in a synthetic fiber spinning process or spinning process and can impart an excellent feeling to a dyed textile product. It is.

[Prior Art] Generally, in order to perform good spinning of synthetic fibers, it is necessary to impart various performances such as antistatic properties, convergence properties, smoothness, and rust prevention properties to synthetic fibers.

In order to improve these performances, various spinning oils in which components for imparting each performance are combined have been used.

For example, as a component that imparts antistatic properties, an alkyl phosphate ester salt, an alkyl sulfate ester salt, a quaternary ammonium compound, a betaine compound, or the like is used.As a component that imparts convergence, polyoxyalkylene phenyl ether, Polyoxyalkylene alkyl ethers, polyoxyalkylene alkyl esters and the like are used. Alkyl alkylates, polyhydric alcohol esters, polyalkylene glycol alkyl esters, paraffins, α-olefins and the like are used as components for imparting smoothness.

[Problems of the Prior Art] However, these conventionally known spinning oils have a narrow application range.

For example, in the knitting process performed after the spinning process, it is necessary to impart performance such as smoothness and flexibility to the fiber, and performance different from that in the spinning process is required. Even if conventional spinning oils are used in the spinning process and exhibit good spinning performance, few of the effects last until the knitting process, and even if they continue, the performance required in the process cannot be satisfied. . Therefore, it is necessary to separately use a knitting oil in the knitting step.

On the other hand, for textile products, the texture of natural fiber products is preferred,
Synthetic fiber products are desired to have the same softness and smoothness of natural fiber products, but conventional spinning oils cannot impart such a feeling, and furthermore, softening agents and smoothing agents It is necessary to use a finishing agent such as an agent.

As described above, conventional spinning oils exhibit performance only in the spinning process and have a narrow range of application, and in order to manufacture synthetic fiber products, various other oils are required, resulting in poor economic efficiency. there were.

The present invention focuses on the above problems, and when used in the spinning or spinning process, satisfies the performance required in each step from the knitting process to the product after dyeing, and provides a good wind. Capable of producing synthetic fiber products having
An object of the present invention is to provide a spinning oil agent for synthetic fibers.

[Means for Solving the Problems] The present inventors have conducted intensive studies in order to solve the above problems, and as a result, have found that alkyl phosphate ester salts, higher fatty acid amide compounds, nonionic surfactants and lower alkanolamines The composition containing the quaternary ammonium salt in a specific manner is used in the spinning process of the synthetic fiber, exhibits each performance required in each process after the spinning process, and has a better feeling. The present invention was found to be an oil agent capable of producing a synthetic fiber product, and led to the present invention.

That is, the present invention relates to (A) alkyl phosphate salt 5 to
80% by weight, (B) 5 to 80% by weight of higher fatty acid amide compound having a total amine value of 30 or less, (C) 5 to 5% of nonionic surfactant
The present invention provides a spinning oil for synthetic fibers, which contains 80% by weight and (D) 3 to 20% by weight of a quaternary ammonium salt of a lower alkanolamine.

The alkyl phosphate ester salt (A) used in the present invention has the following general formula (1) and / or (2) And an alkyl phosphate salt represented by the formula:
In the formulas (1) and (2), R is preferably an alkyl group or an alkenyl group having 4 to 18 carbon atoms, A is an oxyethylene group and / or an oxypropylene group, n is 0 to 10, and m
Is preferably 0 to 3, and X is preferably an alkali metal or an organic amine.

The alkyl phosphate salt is a phosphoric acid ester of an aliphatic alcohol having 4 to 18 carbon atoms and an addition compound obtained by adding 1 to 10 mol of ethylene oxyside or propylene oxide to the aliphatic alcohol, according to a conventional method. After reacting 3 mol or less of ethylene oxide or propylene oxide in accordance with the above, it is obtained by neutralizing with an alkali metal hydroxide or an organic amine compound.

As the aliphatic alcohol used here, butyl alcohol, octyl alcohol, lauryl alcohol,
It is obtained by using aliphatic alcohols having 4 to 18 carbon atoms such as cetyl alcohol, stearyl alcohol, oleyl alcohol, isobutyl alcohol, isooctyl alcohol, isostearyl alcohol, and α-olefins, n-olefins, n-paraffins as raw materials. Synthetic higher alcohols are exemplified, and phosphorus compounds used for the phosphoric esterification reaction include phosphorus pentoxide. In the phosphorylation reaction, a monoalkyl phosphate, a dialkyl phosphate and a mixture thereof are obtained, and any of them can be used. As the alkali metal hydroxide, sodium hydroxide, potassium hydroxide And the organic amine compound includes ammonia, monoethanolamine, diethanolamine, triethanolamine and the like.

The content of the alkyl phosphate salt in the spinning fluid for synthetic fibers of the present invention is 5 to 80%, and 5 to 40% by weight.
Is more preferred. Alkyl phosphate salt content of 5
When the amount is less than the weight%, the antistatic property and the rustproof property are insufficient, and the phenomenon that the fiber is wound around the front roller during spinning or the roller is rusted cannot be prevented. On the other hand, if it exceeds 80% by weight, the antistatic property and the rust-preventing property are improved, but the smoothness between the fiber and the metal is lowered, and the feeling of the obtained fiber product is lowered.

The higher aliphatic amide compound (B) used in the present invention is obtained by performing an amidation reaction according to a conventional method using a polyalkylene polyamine or an alkanolamine and a saturated fatty acid having 10 to 26 carbon atoms. Is a higher fatty acid amide compound having a total amine value of 30 or less, and a compound having a total amine value of 30 or less by reacting urea, epihalohydrin or the like with the higher fatty acid amide compound having a total amine value of 30 or less. Among these amide compounds, those having an amine value can be used after being neutralized with an acid. Examples of the polyalkylene polyamine include ethylene diamine, diethylene triamine, triethylene tetramine,
Examples include tetraethylenepentamine and pentaethylenehexamine. Examples of the alkanolamine include monoethanolamine, diethanolamine, triethanolamine, and N- (2-aminoethyl) -ethanolamine. Examples of the saturated fatty acids having 10 to 26 carbon atoms include lauric acid, myristic acid, palmitic acid, stearic acid, arachiic acid, and behenic acid. These higher fatty acids may be used alone or in combination of two or more. There may be. As higher fatty acids obtained by mixing two or more kinds, fatty acids obtained by decomposing fats and oils such as animal and vegetable fats and oils and hydrogenated hardened fats and the like obtained by hydrogenating these animal and vegetable fats and oils by high-pressure decomposition or lipolytic enzymes according to a conventional method. Is mentioned. The higher fatty acid amide compound has a total amine value of
Those having 30 or less are excellent in compatibility with the alkyl phosphate ester salt, and can give a good feeling to textiles.
If the total amine value exceeds 30, the compatibility with the alkyl phosphate salt is low, which is not preferable, and it is difficult to obtain a stable product and an aqueous solution.

The content of the higher fatty acid amide compound in the synthetic fiber spinning agent of the present invention is 5 to 80% by weight, and more preferably 5 to 40% by weight. Content of higher fatty acid amide compound is 5
If the amount is less than 80% by weight, the effect of imparting a feeling to the fiber product is small, and if it exceeds 80% by weight, it is difficult to prevent the electrification of the fibers, and the convergence between the fibers is not sufficient, and the binding power is insufficient. Absent.

The nonionic surfactant (C) used in the present invention includes polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene styryl ether, polyoxyethylene castor oil ether, polyoxyethylene / polyoxypropylene block. Ether-type nonionic surfactants such as copolymers, sorbitan fatty acid partial esters, glycerin fatty acid partial esters, polyglycerin (polymerization degree 2 to 10) fatty acid partial esters, pentaerythritol fatty acid partial esters, polyethylene glycol fatty acid monoesters or diesters, Fatty acid ester type nonionic surfactants such as polypropylene glycol fatty acid monoesters or diesters, sucrose fatty acid partial esters, etc .; Nonionic surfactant obtained by adding an oxide. The polyoxyethylene group of the ether type nonionic surfactant excluding the polyoxyethylene / polyoxypropylene block copolymer is obtained by adding ethylene oxide, and the number of moles added is preferably 5 to 50 moles. Has preferably 12 to 18 carbon atoms. The polyoxyethylene / polyoxypropylene block copolymer preferably has a molecular weight of 500 to 20,000, and those having the same range of molecular weight are used regardless of the ratio and the order of addition moles of ethylene oxide and propylene oxide. be able to. The fatty acid group of the ester type nonionic surfactant preferably has 12 to 18 oxygen atoms,
The number of moles of ethylene oxide added to the partial ester is preferably 3 to 20 moles.

The content of the nonionic surfactant in the spinning fluid for synthetic fibers of the present invention is 5 to 80% by weight, and more preferably 5 to 40% by weight. If the content is less than 5% by weight, the emulsifying power as an oil agent is weak, and it is difficult to emulsify and use in water.
If it exceeds 80% by weight, the effect of imparting a feeling to the textile by the higher fatty acid amide compound is reduced, and the antistatic property is also reduced.

The spinning oil agent for synthetic fibers of the present invention contains a predetermined amount of the above (A) an alkyl phosphate ester salt, (B) a higher fatty acid amide compound and (C) a nonionic surfactant, and further comprises (D) a lower alkanolamine. By containing a predetermined amount of a quaternary ammonium salt of (A), a very good spinnability can be exhibited and an excellent texture can be imparted to a fiber product. ) The lower alkanolamine quaternary ammonium salt acts synergistically to further enhance the antistatic properties.

The (D) quaternary ammonium salts of lower alkanolamines used in the present invention include lower alkanolamines such as monoethanolamine, diethanolamine, triethanolamine and N- (2-aminoethyl) -ethanolamine in dimethyl sulfate and diethyl sulfate. And quaternary ammonium salts obtained by quaternization.

The content of the quaternary ammonium salt is 3 to 20% by weight. If the content exceeds 20% by weight, the antistatic property is increased, but the rustproofing property is reduced.

The spinning oil agent for synthetic fibers of the present invention comprises: (A) an alkyl phosphate ester salt, (B) a higher fatty acid amide compound,
(C) a nonionic surfactant, and (D) a quaternary ammonium salt of a lower alkanolamine as a main component. If necessary, higher fatty acid alcohol esters, animal and vegetable oils and fats, mineral oils, waxes, silicon compounds Conventionally known softeners and leveling agents can also be blended.
The amount is preferably 20% by weight or less.

The spinning oil agent for synthetic fibers of the present invention can be prepared by mixing predetermined amounts of the above components and dissolving them uniformly.

The synthetic fiber spinning oil agent of the present invention is used in a synthetic fiber spinning process, a method of spinning after treating a synthetic fiber raw yarn with the oil agent, a method of lubricating a fiber being spun, and the like.
Either method can be adopted. Examples of the method for treating the raw yarn include a dipping lubrication method, a roller touch lubrication method, and a spray lubrication method. In refueling, it is preferable to dilute the oil agent with water and use it at a concentration of about 0.01 to 2% by weight.

The spinning oil agent for synthetic fibers of the present invention can be applied to synthetic fibers such as polyacrylonitrile fibers, polyamide fibers, and polyester fibers and polypropylene fibers, and exhibits excellent spinnability particularly when used for polyacrylonitrile fibers and polyamide fibers.

Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to the following examples unless it exceeds the gist.

[Examples] The compounds used in Examples, Reference Examples and Comparative Examples are shown below. An abbreviation is shown in parentheses.

A. alkyl phosphate ester salt (A-1) hydroxyethyl octyl alcohol ether phosphate ester monoethanolamine salt (A-2) octyl alcohol phosphate ester potassium salt (A-3) lauryl alcohol phosphate ester diethanolamine salt (A -4) polyoxyethylene (n = 7) lauryl alcohol ether phosphate sodium salt (A-5) octyl alcohol phosphate monoethanolamine salt (A-6) cetyl alcohol phosphate ester potassium salt B. higher fatty acid Amide Compound The higher fatty acid amide compound used was synthesized as shown below.

A higher fatty acid and a polyalkylene polyamine or an alkanolamine shown in Table 1 are charged at a predetermined ratio into a reaction vessel equipped with a stirrer, and a dehydration reaction is performed at 170 to 200 ° C. for 6 hours under a nitrogen gas stream to obtain a higher fatty acid amide compound ( B-1, 3,
7) was obtained. After the same amide reaction was further performed, predetermined amounts of urea and epichlorohydrin were added, and the mixture was heated at 90 to 130 ° C for 1 hour.
~ 2 hours reaction, higher fatty acid amide compound B-2,
4-6 were obtained. Table 1 shows the synthesis conditions, total amine value, and abbreviations for each compound.

C / nonionic surfactant (C-1) polyoxyethylene (n = 7) lauryl ether (C-2) polyoxyethylene (n = 25) cetyl ether (C-3) polyoxyethylene (n = 25) castor oil ether (C-4) polyoxyethylene (n = 20) nonylphenyl ether (C-5) polyoxyethylene (n = 20) sorbitan monolauryl ester ( C-6) Polyethylene glycol (MW400) dilaurate D. Quaternary ammonium salt of lower alkanolamine (D-1) N- (2-aminoethyl) ethanol diethyl sulfate (D-2) monoethanolamine dimethyl sulfate ( D-3) Diethanolamine diethyl sulfate (D-4) Diethynolamine dimethyl sulfate (D-5) Triethanolamine dimethyl sulfate E. Other additives (E-1) Stearic acid butyl ester (E-2) Paraffin Wax (melting point: 60 ° C.) (E-3) Octyl stearate Examples 1-4, Comparative Examples 1-5 Raw materials A-E shown in Table 2 were charged in a predetermined amount into a mixing pot,
Heat to 90 ° C, gradually add warm water at the same temperature to emulsify,
An emulsified liquid having a concentration of% by weight was prepared and subjected to a test. Table 2 shows the types, blending ratios, and emulsion stability of the raw materials used in the preparation of each synthetic fiber spinning oil. In the table, the two-stage writing of the components A to D of the “spinning oil composition” in each example is a mixture of two types, and the numerical value in parentheses indicates the mixing ratio (%). Then, A-1 is 25%, B-3 is 20% and B-4 is
20%, C-1 25%, C-5 5%, and D-1 5%
It shows that they are used together.

Next, 5 kg of acrylic soup (2d x 51 mm) is 1% of the above oil
After immersion in an aqueous solution (liquid temperature 60 ° C, 1 minute), use a centrifugal dehydrator to adjust the impregnation amount of the oil solution to 1.5 kg,
The oil was dried at 1 ° C. for 1 hour to perform oiling treatment (oiling rate after drying was 0.3% by weight). The lubricated acrylic swoof was spun (opening step-carding step-roughing step-spinning step) according to a conventional method to obtain a 1 / 40th spun yarn, and at the same time the spinnability was evaluated. Further, using the obtained spun yarn, the feeling, the feeling after dyeing, and the knitting property were evaluated. Table 2 shows the evaluation results of each performance.

・ Evaluation test of spinning performance The amount of static electricity generated in the spinning process, winding around a continuous roller, and yarn breakage during spinning were measured to evaluate spinning performance.

The amount of generated static electricity: The amount of generated static electricity on the card web in the carding process was measured using a current collecting potential meter manufactured by Kasuga Electric Co., Ltd.

Winding around the continuous roller: The state of the front roller of the spun sliver in the continuous step was visually observed and evaluated.

Spinning: The number of yarn breaks in the spinning process was measured and evaluated according to the following criteria.

◎: No thread breakage in spinning process ○: Almost no thread breakage in spinning process △: Slight thread breakage in spinning process ×: Many thread breakage in spinning process ・ Hand evaluation test Handling of 10 panelists The hand of the spun yarn and the dyed yarn was evaluated according to the following criteria.

 ：: Very good flexibility of the yarn ○: Good flexibility of the yarn △: Slightly hard and slightly inferior in flexibility ×: Dyed yarn is hard, has a feeling of creaking, and has poor flexibility In addition, dyeing of spun yarn Was subject to the following conditions:

Dyeing material: CATHILONRED GCLH manufactured by Hodogaya Chemical Co., Ltd.
1.0% owf buffering agent: Ospin AN 1.0% owf pH adjusting agent: acetic acid 0.5% owf sodium acetate 0.5% owf-Knitting property evaluation test Knitted spun yarn was evaluated under the following conditions.

Measuring machine: Sugihara Keiki knitting tester Condition Atmosphere: 25 ° C, 40% RH Yarn speed: 50cm / min, 100m / min Yarn-metal friction: 3 18-gauge knitting needles, 3 places Yarn-yarn friction : Twice two twists One twist one place [Effects of the Invention] As described above, the spinning for synthetic fibers of the present invention. The oil agent contains an alkyl phosphate ester salt, a higher fatty acid amide compound, a nonionic surfactant and a quaternary ammonium salt of a lower alkanolamine in a specific ratio, and is used in a spinning process or a spinning process of a synthetic fiber. It exhibits good spinnability and spinnability, and can impart an excellent texture to textile products after dyeing, and simplifies the process as compared to conventional methods using many types of process oils. It has the effect of being able to do so.

Continuation of the front page (58) Field surveyed (Int.Cl. ⁶ , DB name) D06M 13/00-13/535 D06M 15/00-15/715

Claims (1)

(57) [Claims] (A) 5-80% by weight of an alkyl phosphate ester salt; (B) 5-80% by weight of a higher aliphatic amide compound having a total amine value of 30 or less; A spinning oil agent for synthetic fibers, comprising 80% by weight and (D) 3 to 20% by weight of a quaternary ammonium salt of a lower alkanolamine.