JP4755313B2 - Method for producing polyester dyed fiber and scouring dyeing assistant - Google Patents

Description

  The present invention relates to a method for producing a polyester dyed fiber, and a scouring dyeing assistant suitably used in this method.

In general, dyeing of polyester fibers is performed by sufficiently scouring and dyeing a dyed object using a disperse dye in a weakly acidic region under a high temperature and high pressure of 110 to 140 ° C. At this time, a disperse leveling agent is added to the dyeing bath in order to help the dispersibility of the disperse dye and further promote the slow dyeing effect or the transfer effect to improve the level dyeing property.
If the material to be dyed has undergone a scouring process, there is no problem even if a normal dyeing method is used, but if the scouring is insufficient or unscoured, the fiber oil adhering to the material to be dyed is a disperse dye. Since the dispersibility is lowered, specs of disperse dyes are easily generated, troubles such as stains on dyed articles and contamination of cans of dyeing machines occur, and conventional dyeing methods cannot be used.

  Further, in recent dyeing processing, in order to meet various demands, there is a tendency to make a large variety of small lots, and processing costs are rising. Therefore, the machining process is being shortened or simplified to reduce the machining cost. In particular, when improvement of productivity and energy saving are considered, means for simplifying or omitting the scouring step and the cleaning step have been taken. Therefore, the fiber oil agent etc. that should have been removed in the scouring process will enter the dyeing process while remaining in the dyed object. Problems such as contamination of cans have become a major problem.

  In order to solve such problems, methods described in Patent Document 1 and Patent Document 2 have been proposed. The method described in Patent Document 1 uses a pH slide agent and changes the staining solution from alkaline to acidic so as to scour it in an alkaline state and dye it in an acidic state. However, in this method, it is difficult to adjust the amount of the pH slide agent added, and there is a concern that the free acid of the pH slide agent binds to a divalent metal component such as calcium or magnesium to generate scale. The method described in Patent Document 2 is intended to enhance the scouring effect in alkali dyeing. However, alkali dyeing is not versatile because it has less dye species and is more expensive than disperse dyes that are usually used in an acidic manner.

JP-A-60-224884 Japanese Patent Laid-Open No. 3-90686

  In view of the background art, an object of the present invention is to disperse unscoured or insufficiently scoured polyester fibers with a disperse dye, and to perform a scouring and dyeing process in a single bath. It is an object of the present invention to provide a method for producing a polyester-based dyeing fiber that suppresses the generation of specs and suppresses stains on a dyed product and contamination of a can of a dyeing machine, and a scouring dyeing assistant that can be suitably used in this method.

As a result of intensive investigations to solve the above problems, the present inventors have scoured in one bath as long as it is a method for producing a polyester-based dyed fiber using a specific nonionic surfactant and a specific anionic surfactant. It has been found that the dyeing process can be performed, the generation of the spec of the disperse dye is suppressed, and good scouring properties are imparted to the dyed product.
That is, the present invention is a raw material polyester comprising a nonionic surfactant (A) represented by the following general formula (1), an anionic surfactant (B) represented by the following general formula (2) and a disperse dye. This is a method for producing a polyester-based dyeing fiber, in which a scouring and dyeing process is performed on the fiber.

（式中、Ａ^１Ｏは、炭素数２〜４のオキシアルキレン基であり、ｎは２〜５０の整数であり、ｐは１または２である。）

(In the formula, A ¹ O is an oxyalkylene group having 2 to 4 carbon atoms, n is an integer of 2 to 50, and p is 1 or 2.)

（式中、Ａ^２Ｏは、炭素数２〜４のオキシアルキレン基であり、ｍは２〜５０の整数であり、ｑは１または２であり、Ｍは水素原子、アルカリ金属、アルカリ土類金属、アンモニウム、４級アンモニウム、アルキルアミンまたはアルカノールアミンである。）

(In the formula, A ² O is an oxyalkylene group having 2 to 4 carbon atoms, m is an integer of 2 to 50, q is 1 or 2, and M is a hydrogen atom, an alkali metal, or an alkaline earth. Metal, ammonium, quaternary ammonium, alkylamine or alkanolamine.)

The treatment is particularly suitable when performed under acidic conditions. The pH of the bath (25 ° C.), that is, the pH (25 ° C.) of the bath when scouring and dyeing the raw material polyester fiber is preferably 3-6.
The weight ratio (A / B) of the nonionic surfactant (A) to the anionic surfactant (B) in the bath is preferably 95/5 to 20/80. The concentration of the nonionic surfactant (A) is preferably 0.01 to 80 g / L, and the concentration of the anionic surfactant (B) in the bath is preferably 0.01 to 70 g / L.
Moreover, it is preferable that the temperature at the time of performing the said process is 80-180 degreeC.

Further, in the method for producing a polyester-based dyed fiber of the present invention, the bath further contains a flame retardant, and in addition to the treatment, the treatment for flame retardant processing can be performed in one bath.
Moreover, in the method for producing a polyester-based dyed fiber of the present invention, the bath further includes a light-resistant agent, and in addition to the treatment, the light-resistant processing can be performed in one bath.

The polyester fiber scouring dyeing assistant of the present invention includes a nonionic surfactant (A) represented by the above general formula (1) and an anionic surfactant (B) represented by the following general formula (2). It is used for scouring and dyeing in a bath.
The weight ratio (A / B) of the nonionic surfactant (A) to the anionic surfactant (B) in the scouring dyeing assistant is preferably 95/5 to 20/80.
The weight ratio of the nonionic surfactant (A) in the nonvolatile content of the scouring dyeing assistant is 20 to 95% by weight, and the weight ratio of the anionic surfactant (B) is 5 to 80% by weight. preferable.

  The method for producing a polyester-based dyed fiber according to the present invention allows a scouring and dyeing process to be performed in one bath when dyeing unscoured or insufficiently sewed polyester fiber with a disperse dye. The generation of specs can be suppressed, and stains on the dyed product and can contamination of the dyeing machine can be suppressed. Moreover, according to the manufacturing method of this invention, the polyester dyeing fiber which has favorable scouring property and dyeability can be obtained. The scouring and dyeing assistant of the present invention is used for scouring and dyeing in one bath, and exhibits the same effect.

  The method for producing a polyester-based dyed fiber of the present invention includes a nonionic surfactant (A) represented by the general formula (1), an anionic surfactant (B) represented by the general formula (2), and a disperse dye. The raw polyester fiber is scoured and dyed in one bath. This will be described in detail below.

[Nonionic surfactant (A)]
The nonionic surfactant (A) represented by the general formula (1) is a component that is essential in the bath for scouring and dyeing the raw material polyester fiber without inhibiting the dispersion of the disperse dye, Can disperse fiber oil adhering to the raw material polyester fiber, and by using together with anionic surfactant (B) described later in one bath, it is possible to suppress the generation of disperse dye specifications and to impart good scouring properties to the dyed product .
In the general formula (1), A ¹ O is an oxyalkylene group having 2 to 4 carbon atoms, and may be one type or two or more types. In the case of two or more types, any of a block adduct, an alternating adduct, or a random adduct may be configured. Among these, an oxyethylene group and an oxypropylene group are preferable and an oxyethylene group is more preferable because the dispersibility of the fiber oil agent is excellent as the number of carbon atoms is small.
n is an integer of 2 to 50, preferably 3 to 40, more preferably 5 to 30, and still more preferably 10 to 30. When n is less than 2, the hydrophilicity becomes too low and the dispersibility of the fiber oil agent is poor. On the other hand, when it exceeds 50, the hydrophilicity becomes too high and the dispersibility of the fiber oil agent is poor.
p is 1 or 2. When p is 3 or more, the dispersion of the disperse dye is affected, and the dispersibility of the fiber oil agent is lowered. p is preferably 1 because the dispersibility of the fiber oil agent is excellent.
1 type (s) or 2 or more types may be used for a nonionic surfactant (A).

[Anionic surfactant (B)]
The anionic surfactant (B) represented by the general formula (2) is also a component that is essential in the bath for scouring and dyeing the raw material polyester fiber, and is dispersed without being affected by the fiber oil. The dye can be dispersed, and by using it together with the above-described nonionic surfactant (A) in one bath, the generation of the spec of the disperse dye can be suppressed and good scouring properties can be imparted to the dyed product.
In the general formula (2), A ² O is an oxyalkylene group having 2 to 4 carbon atoms, and may be one or more. In the case of two or more types, any of a block adduct, an alternating adduct, or a random adduct may be configured. Among these, an oxyethylene group and an oxypropylene group are preferable, and an oxyethylene group is more preferable because the dispersibility of the disperse dye is excellent as the number of carbon atoms is small.
m is an integer of 2 to 50, preferably 3 to 40, more preferably 5 to 35, and still more preferably 6 to 30. When m is less than 2, the proportion of —SO ₃ M in the molecule becomes too large, and the dispersibility of the disperse dye is poor. On the other hand, if it exceeds 50, the proportion of —SO ₃ M in the molecule becomes too small, and the dispersibility of the disperse dye is poor.
q is 1 or 2. When q is 3 or more, it is affected by the fiber oil agent, and the dispersibility of the disperse dye is lowered, which is not preferable. q is preferably 2 because the dispersibility of the disperse dye is excellent.

M is a hydrogen atom, an alkali metal, an alkaline earth metal, ammonium, a quaternary ammonium, an alkylamine or an alkanolamine. Examples of the alkali metal include sodium, potassium, lithium and the like. Examples of the alkaline earth metal include magnesium, calcium, and barium. Examples of quaternary ammonium include tetramethylammonium, tetraethylammonium, tetramethanolammonium, and tetraethanolammonium. 1-20 are preferable, as for carbon number of alkanolamine, 1-10 are more preferable, and 1-6 are more preferable. Examples of the alkanolamine include methanolamine, ethanolamine, dimethanolamine, diethanolamine, trimethanolamine, and triethanolamine. Among these, a hydrogen atom, an alkali metal, ammonium, or an alkanolamine is more preferable because of increasing the water solubility.
An anionic surfactant (B) may use 1 type (s) or 2 or more types.

[Disperse dye]
The dye used in the method for producing the polyester-based dyed fiber of the present invention is a disperse dye, and in addition to the nonionic surfactant (A) and the anionic surfactant (B), the raw polyester fiber is scoured and dyed. It is a component contained in one bath for processing. Although there are disperse dyes that can be used under alkaline conditions, disperse dyes that can be used under acidic conditions are preferred in the present invention.
In general, fiber oil agents are technically more difficult to disperse under acidic conditions than under alkaline conditions. Therefore, when dyeing unscoured or insufficiently scoured polyester fibers with disperse dyes under acidic conditions, the fiber oil agent cannot be removed from the fiber, or the fiber oil agent is poorly dispersible in the dye bath. There is a high possibility that In the case of poor scouring in which the fiber oil agent cannot be removed from the fiber, the fiber oil agent remains in the post-processing step, so that the adhesion of the processing agent is lowered and the performance of the processing agent may be lowered. In addition, when the fiber oil agent is in a poorly dispersible state in the dyeing bath, the fiber oil agent reduces the dispersibility of the disperse dye, causing speculation of the disperse dye, causing stains on the dyed product and the can of the dyeing machine. Troubles such as contamination occur.

  The disperse dye is not particularly limited, and known dyes can be used. For example, Sumikaron dye, Kayalon Polyester dye, Miketon Polyester dye, Palanil dye, Dianix dye, TD dye, Kiwalon Polyester dye, Terasil dye, Foron dye, Serilene dye and the like can be mentioned.

[Flame Retardant, Light Resistant]
In order to simplify and shorten the process, the exhausting treatment of the flame retardant and the light proofing agent may be performed simultaneously in the dyeing bath. When scouring and dyeing in a single bath, the conventional technology not only generates disperse dye specifications but also agglomerates flame retardants and light-proofing agents, causing problems such as stains on dyed products and stains on dyeing machine cans. There was a risk of causing it. Moreover, if such agglomerates are produced in large quantities, there is a risk of inducing a decrease in flame retardancy and light resistance of the dyed product.
If it is the manufacturing method of the polyester dyeing fiber of this invention, since aggregation of a flame retardant and a light-resistant agent can also be suppressed, in addition to processing of scouring and dyeing in one bath, a flame retardant and a light-resistant agent are also simultaneously performed. It is possible to perform exhaustion treatment. That is, the method for producing a polyester-based dyed fiber of the present invention includes a flame retardant and / or a light resistance agent in a bath containing a nonionic surfactant (A), an anionic surfactant (B) and a disperse dye, In addition to the dyeing process, the flame-retardant process and / or the light-resistant process can be performed in one bath.

  The flame retardant is a substance having flame retardancy and is not particularly limited as long as it can be treated simultaneously in a dye bath, and a known one can be adopted. Examples of the flame retardant include (trimethyl phosphate, triethyl phosphate, tributyl phosphate, tri (2-ethylhexyl) phosphate, phenyl (2-ethylhexyl) mixed phosphate, triphenyl phosphate, tricresyl phosphate, trixylenyl phosphate, triisopropyl Phenyl phosphate, tri-t-butylphenyl phosphate, cresylphenyl mixed phosphate, isopropylphenylphenyl mixed phosphate, t-butylphenylphenyl mixed phosphate, xylenylphenyl mixed phosphate, cresylxylenyl mixed phosphate, phenyl orthoxenyl mixed Phosphate esters such as phosphate and naphthylphenyl mixed phosphate; hydroquinone bis (diphenyl phosphate ), Resorcinol bis (dicresyl phenyl phosphate), resorcinol bis (diphenyl phosphate), bisphenol A bis (diphenyl phosphate), bisphenol A bis (dicresyl phosphate), bisphenol A bis (dixylenyl phosphate), resorcinol bis (dixile) Nyl phosphate), bisphenol S bis (diphenyl phosphate), bisphenol S bis (dicresyl phosphate), condensed phosphate esters such as bisphenol S bis (dixylenyl phosphate); phosphite esters; 10-benzyl-9,10- Hypophosphites such as dihydro-9-oxo-10 (5) -phosphaphenanthrene = 10-oxide; triphenylphosphine oxide, tris (2-methylphenyl) phos Oxide, tris (4-methylphenyl) phosphine oxide, tris (2,6-dimethylphenyl) phosphine oxide, tris (2,6-dimethoxyphenyl) phosphine oxide, tribenzylphosphine oxide, 2- (diphenylphosphinyl) hydroquinone Phosphine oxides such as diphenylphenylamide phosphate, phenylbis (phenylamide) phosphate, etc .; Chlorine-containing phosphate ester; Chlorine-containing condensed phosphate ester; Phosphorus-containing polyester resin; Triphenoxytrimethoxycyclotriphosphazene, Phosphazenes such as hexaphenoxycyclotriphosphazene; hexabromocyclododecane, decabromodiphenyl ether, ethylenebis (pentabromodiphenyl), Examples thereof include brominated flame retardants such as ethylenebis (tetrabromophthalimide), tris (tribromophenoxy) triazine, and tris (2,3-dibromopropyl) isocyanurate.

  The light resistance agent is a substance having light resistance and is not particularly limited as long as it can be simultaneously processed in a dyeing bath, and a known one can be adopted. Examples of the light fastener include (2- (2′-hydroxy-3′-t-butyl-5′-methylphenyl) -5-chlorobenzotriazole, 2- (2′-hydroxy-5′-methylphenyl)). Benzotriazole ultraviolet absorbers such as benzotriazole; benzophenone ultraviolet absorbers such as 2-hydroxy-4-methoxybenzophenone and 2,2 ′, 4,4′-tetrahydroxybenzophenone; 2- (4,6-diphenyl- 1,3,5-triazin-2-yl) -5- (hexyloxy) -phenol, 2,4-bis (2,4-dimethylphenyl) -6- (2-hydroxy-4-octyloxyphenyl)- Triazine ultraviolet absorbers such as 1,3,5-triazine; Benzoxa such as 2,2 ′-(p-phenylene) di-3,1-benzoxazin-4-one Non-based ultraviolet absorbers; Cyanoacrylate-based ultraviolet absorbers such as ethyl-2-cyano-3,3-diphenyl acrylate and (2-ethylhexyl) -2-cyano-3,3-diphenyl acrylate; p-t-butylphenyl Examples thereof include salicylate-based ultraviolet absorbers such as salicylate.

[Other ingredients]
The bath in which the scouring and dyeing processes are performed contains water in addition to the nonionic surfactant (A), the anionic surfactant (B) and the disperse dye. The water used in the present invention may be any of pure water, distilled water, purified water, soft water, ion exchange water, tap water and the like.
Moreover, you may contain other components other than this in the range which does not impair the effect of this invention. Examples of other components include a pH adjuster, an antifoaming agent, a solvent, and a fatty acid (salt). Examples of the pH adjuster include acetic acid, sodium acetate, lactic acid, sodium lactate, phosphoric acid, sodium dihydrogen phosphate, disodium hydrogen phosphate, and trisodium phosphate.

[Raw material polyester fiber]
The raw material polyester fiber used in the present invention is not particularly limited, and may be any shape such as knitted fabric, woven fabric, cheese, and skein. Among these, a knitted fabric is preferable because it is suitable for a liquid flow dyeing apparatus.
Further, as the raw material polyester fiber used in the present invention, unrefined or insufficiently refined polyester fiber is preferable. In general, a polyester-based fiber is attached with a spinning oil provided at the time of spinning, a weaving oil provided at the time of weaving, a glue, a knitting oil provided at the time of knitting, and the like. In the method for producing a polyester-based dyed fiber of the present invention, it can be particularly preferably used in the case of unscoured or insufficiently scoured polyester fiber to which a fiber oil composed of a spinning oil and / or a knitting oil is adhered. Specifically, the raw material polyester fiber to which 0.5% by weight or more of the fiber oil agent is attached to the entire polyester fiber is preferable.
There is no limitation in particular as a textile oil agent, The well-known thing generally used is mentioned. Examples thereof include mineral oil, paraffin, hardened oil, ester oil, silicone oil, nonionic surfactant, anionic surfactant, and cationic surfactant.

  (Raw material) The polyester fiber means a polyester fiber or a fiber in which a polyester fiber is combined, and the polyester fiber is not only polyethylene terephthalate fiber but also polylactic acid (PLA) fiber, polytrimethylene terephthalate (PTT) fiber, It means a fiber made of a polymer condensed by a reaction forming an ester bond, such as polybutylene terephthalate (PBT) fiber, polyethylene naphthalate (PEN) fiber, or polyarylate fiber. Examples of the fiber combined with the polyester fiber include cellulose fiber, polyamide fiber, and polyurethane fiber.

[Production method of polyester dyed fiber]
The polyester dyed fiber production method of the present invention is a method in which the raw polyester fiber is scoured and dyed in one bath, and the bath is composed of the above-mentioned nonionic surfactant (A), the above-mentioned anionic surfactant ( B) and disperse dyes. That is, a scouring process and a dyeing process are simultaneously performed in a single bath. The production method of the present invention can be applied to all dye fiber dyeing operations.
As a method for producing the polyester-based dyed fiber of the present invention, first, a nonionic surfactant (A), an anionic surfactant (B), a disperse dye and water are introduced into a bath at a predetermined ratio and mixed and stirred. Then, a pH adjusting agent is added to adjust to a predetermined pH (25 ° C.) to prepare a scouring / dyeing solution in one bath. The nonionic surfactant (A) and the anionic surfactant (B) may be added individually into the bath, or may be added as a scouring dyeing aid for the polyester fibers described later.
Next, the raw material polyester fiber is put into the bath, and then the scouring / dyeing solution is heated to a predetermined dyeing temperature and held at that temperature for 10 to 60 minutes to penetrate the disperse dye into the polyester fiber. , Dye. At that time, scouring is also performed at the same time. After the scouring / dyeing process, the dyeing solution is discarded and washed with hot water, washed with water, or reduced for the purpose of washing away unfixed disperse dyes. Then, it is made to dry and a polyester dyeing fiber can be obtained.
The polyester dyed fiber obtained by such a production method has good scouring properties and dyeability.

The pH (25 ° C.) of the bath when scouring and dyeing the raw material polyester fiber is preferably 3 to 6, and preferably 3.5 to 5.5. In the production method of the present invention, scouring and dyeing can be simultaneously performed on the acidic side, and a process of adjusting to the acidic side when dyeing is unnecessary as in Patent Document 1 without using an alkaline side. It is. Moreover, a pH slide agent is unnecessary, and there is no concern that the free acid of the pH slide agent binds to a divalent metal component such as calcium or magnesium to generate scale.
Moreover, the dyeing | staining temperature at the time of processing a raw material polyester-type fiber in a bath (scouring process and dyeing | staining process) is preferable 80-180 degreeC, 90-150 degreeC is preferable, 100-150 degreeC is more preferable, 110-140 More preferably. In the present invention, as in Patent Document 1, in order to adjust the pH (shift from scouring treatment to dyeing treatment), it is not necessary to adjust the treatment temperature in two stages so as to increase the bath temperature.

Further, the method for producing a polyester-based dyed fiber of the present invention includes a flame retardant and / or a light fastness agent in a bath containing the above-described nonionic surfactant (A), anionic surfactant (B), and disperse dye, In addition to the dyeing process, the flame-retardant process and / or the light-resistant process can be performed in one bath.
In the production method of the present invention in which flame retardant processing and / or light resistance processing is performed, a chemical (water dispersion) in which the above-mentioned flame retardant and / or light resistance is dispersed in water is usually used. There are no particular limitations on the method for preparing these drugs, and known techniques can be employed. The weight ratio of the flame retardant to the whole drug is preferably 1% to 99% by weight, more preferably 5 to 80% by weight, and further preferably 10 to 60% by weight. The weight ratio of the light-proofing agent to the whole drug is preferably 1% by weight to 99% by weight, more preferably 5 to 80% by weight, and further preferably 10 to 60% by weight.

  When preparing the scouring / dye solution, such a chemical is put into the bath simultaneously with the nonionic surfactant (A), the anionic surfactant (B), the disperse dye and water, and the raw polyester fiber at the dyeing temperature. The flame retardant and / or light proofing agent is exhausted (flame retardant processing and / or light proof processing). Since the exhausting process and the scouring / dying process are performed simultaneously, the exhausting process conditions are the same as the above-described scouring / dying process conditions.

The concentration of the nonionic surfactant (A) in the treatment bath is preferably 0.01 to 80 g / L, more preferably 0.1 to 60 g / L, and still more preferably 0.2 to 40 g / L. If it is less than 0.01 g / L, the dispersibility of the fiber oil may be insufficient. On the other hand, if it exceeds 100 g / L, it may not be economically preferable.
The concentration of the anionic surfactant (B) in the treatment bath is preferably 0.01 to 70 g / L, more preferably 0.1 to 60 g / L, and still more preferably 0.2 to 50 g / L. If it is less than 0.01 g / L, the dispersibility of the disperse dye may be insufficient. On the other hand, if it exceeds 70 g / L, it may be economically undesirable.
The weight ratio (A / B) between the nonionic surfactant (A) and the anionic surfactant (B) in the treatment bath is 95/95 from the viewpoint of establishing superior dispersion performance of both the fiber oil agent and the disperse dye. 5/20/80 is preferable, 85 / 15-30 / 70 is more preferable, 80 / 20-35 / 65 is further more preferable, and 75 / 25-40 / 60 is particularly preferable.

  Further, it is preferable that the bath in which the scouring and dyeing processes are performed does not contain a temperature conversion type pH slide agent (at least one carboxylic acid ester selected from monovalent, divalent and polyvalent carboxylic acid esters). Specifically, the concentration of the temperature conversion type pH slide agent is preferably 1 g / L or less, more preferably 0.5 g / L or less, and further preferably 0.1 g / L or less.

  The weight ratio of the raw material polyester fiber in the treatment bath (bath ratio = fiber weight: treatment liquid weight) is preferably 1: 3 to 1:60, more preferably 1:40 to 1: 4, and 1: 5. ~ 1: 20 more preferred. When the ratio is less than 1: 3, the circulation of the treatment bath liquid is deteriorated, and the scourability may not be sufficiently exhibited. When the ratio exceeds 1:50, the amount of the treatment bath liquid is large relative to the fiber to be treated, which is not efficient.

  The concentration of the disperse dye in the treatment bath is preferably 0.01 to 50% by weight (on weight of fiber), more preferably 0.1 to 40% by weight of owf with respect to the raw material polyester fiber to be charged. 0.2 to 30% by weight owf is more preferable.

The concentration of the flame retardant in the treatment bath is preferably 0.01 to 50% by weight owf, more preferably 0.1 to 40% by weight owf, and further preferably 0.2 to 30% by weight owf.
The concentration of the light resisting agent in the treatment bath is preferably 0.01 to 50% by weight owf, more preferably 0.1 to 40% by weight owf, and further preferably 0.2 to 30% by weight owf.

Examples of the method for producing the polyester dyed fiber of the present invention include the following. First, the nonionic surfactant (A) of the present invention, the above-mentioned anionic surfactant (B), disperse dye and water are put into a dyeing machine, mixed and stirred, and then a pH adjuster is added to adjust the pH to 4. Adjust to 5 to prepare a scouring / dyeing solution for one bath. Next, the raw polyester fibers are put into a dyeing machine filled with a scouring / dyeing solution, and the temperature of the scouring / staining solution is increased to 135 ° C at a rate of 2 ° C per minute while the scouring / dying solution is convected. Warm up. When the temperature reaches 135 ° C., this temperature is maintained and the scouring / staining solution is convected for 30 minutes. Then, it cools and drains at 70 degreeC, and it supplies water again and performs the water washing process for 5 minutes. This water washing treatment is repeated once more, and after draining, the polyester fiber is dried to obtain the polyester dyed fiber of the present invention.
In addition, in the manufacturing method of the polyester dyeing fiber of this invention, there is no limitation in particular about processes / methods other than the above-mentioned, A well-known process / method is employable.

[Scouring dyeing assistant]
The polyester fiber scouring dyeing assistant of the present invention comprises a nonionic surfactant (A) represented by the above general formula (1) and an anionic surfactant (B) represented by the above general formula (2). Used for scouring and dyeing in one bath. The scouring dyeing assistant of the present invention is suitably used in the method for producing a polyester dyed fiber of the present invention. The nonionic surfactant (A) and the anionic surfactant (B), which are essential components of the scouring dyeing assistant, are as described above.

  Examples of other components contained in the scouring dyeing assistant include water, solvents, antifoaming agents, and alkali agents. The water may be pure water, distilled water, purified water, soft water, ion exchange water, tap water or the like. Examples of the solvent include methanol, ethanol, propanol, butanol, ethylene glycol, propylene glycol, ethyl cellosolve, butyl cellosolve, and solfit. Examples of antifoaming agents include silicone antifoaming agents, mineral oil defoaming agents, polyether antifoaming agents, and fatty acid (salt) antifoaming agents.

The weight ratio of the nonionic surfactant (A) in the nonvolatile content of the scouring dyeing assistant is preferably 20 to 95% by weight, more preferably 30 to 85% by weight, and still more preferably 40 to 75% by weight. Moreover, 5 to 80 weight% is preferable, as for the weight ratio of the anionic surfactant (B) to the non volatile matter of a scouring dyeing assistant, 15 to 70 weight% is more preferable, and 25 to 60 weight% is further more preferable. In addition, the non-volatile matter as used in the field of this invention means the residual component when a scouring dyeing assistant is heat-processed at 105 degreeC for 15 minutes, and a solvent etc. are volatilized.
The weight ratio (A / B) of the nonionic surfactant (A) to the anionic surfactant (B) in the scouring dyeing assistant is 95 from the viewpoint of establishing better dispersion performance of both the fiber oil agent and the disperse dye. / 5-20 / 80 is preferable, 85 / 15-30 / 70 is more preferable, 80 / 20-35 / 65 is further more preferable, and 75 / 25-40 / 60 is particularly preferable.
The weight ratio of the non-volatile component in the scouring dyeing assistant is preferably 10 to 90% by weight, more preferably 20 to 85% by weight, and still more preferably 30 to 80% by weight.

  The method for producing the scouring dyeing assistant of the present invention is not particularly limited, and a known method can be employed. For example, there may be mentioned a method in which each component constituting the scouring dyeing assistant is introduced into water and mixed with stirring.

  EXAMPLES Hereinafter, examples of the present invention will be shown and the present invention will be described in more detail. However, the present invention is not limited to these examples. In the examples, “parts” and “%” represent “parts by weight” and “% by weight”, respectively.

Example 1
As shown in Table 1, 30 parts by weight of POE (15 mol) monostyrenated phenol as nonionic surfactant (A) and 30 parts by weight of POE (10 mol) distyrenated phenol sulfate Na as anionic surfactant (B) Then, 5 parts by weight of palm oil fatty acid K salt and 35 parts by weight of water were mixed and stirred to obtain a scouring dyeing assistant.
Next, a scouring dyeing assistant is added to a mini-color dyeing pot filled with water to a concentration of 1 g / L, followed by Kaylon Polyester Black RV-SF300 (3 wt% owf, Nippon Kayaku Co., Ltd.) ) Was dissolved in water at 30 to 35 ° C., and then adjusted to pH 4.5 with acetic acid / sodium acetate buffer to prepare a scouring dyeing bath.
Next, it is put into a scouring and dyeing bath in which a polyester tropical living machine having an oil landing amount of 1.1% by weight (oil receiving component: mineral oil 1.0% by weight, nonionic surfactant 0.1% by weight) is prepared. And processed in mini color. The bath ratio at that time was 1:15. As processing conditions, the temperature was raised to 135 ° C. at a rate of 2 ° C. per minute and maintained at 135 ° C. for 30 minutes. Then, when it cooled and became 70 degreeC, the scouring dyeing bath was discarded and it washed with water for 5 minutes.
Next, the fiber was dehydrated with a centrifugal separator and dried at 90 ° C. for 1 hour to obtain a target polyester dyed fiber.
The scourability and dyeability of the obtained polyester dyed fibers were evaluated by the following methods. The results are shown in Table 3.

<Scourability>
About the obtained polyester dyed fiber, it extracted for 1 hour with the Soxhlet extraction apparatus using n-hexane, and the amount of residual fat was measured. The amount of residual fat here refers to the weight% extracted with respect to the polyester dyed fiber. Under these conditions, the residual fat amount is desirably 0.25% by weight or less.
<Dyeability>
The presence or absence of dyeing spots on the obtained polyester dyed fibers was visually evaluated according to the following criteria.
○: Less than 10% of the spots where dyeing spots appear on the dyed fibers.
Δ: Dyeing spots are 10% or more and less than 40% on the dyed fiber.
X: The dyeing spot generation | occurrence | production site | part is 40% or more on dyed fiber.

<Prevention of specs>
For anti-specs properties, the scouring dyeing assistant prepared above was put in a mini-color dedicated dyeing pot filled with water to a concentration of 1 g / L, and then Kaylon Polymer Black RV-SF300 (3 wt. % Owf, manufactured by Nippon Kayaku Co., Ltd.) was dissolved in water at 30 to 35 ° C., and adjusted to pH 4.5 with an acetic acid / sodium acetate buffer to prepare a scouring dyeing bath. Thereafter, Brian C-1800 (2 g / L, manufactured by Matsumoto Yushi Seiyaku Co., Ltd.) was added as a knitting oil into the bath. The assumed bath ratio at that time was 1:15.
Next, only the scouring dyeing bath was treated with a mini color. As processing conditions, the temperature was raised to 135 ° C. at a rate of 2 ° C. per minute and maintained at 135 ° C. for 30 minutes. Then, when it cooled and became 30 degreeC, the scouring dyeing liquid was filtered using the filter paper. The evaluation was performed according to the following criteria with the filter paper naturally dried.
○: Almost no color on filter paper.
×: Specs exist on the entire surface of the filter paper, and intense coloration is observed on the filter paper (equivalent to the case of filtering a scouring dyeing solution obtained by treating a blank (BL, Comparative Example 7) not containing a scouring dyeing aid with a mini color) .
Δ: Specs exist on the entire surface of the filter paper, and the filter paper is colored (intermediate level between ◯ and ×).

(Examples 2-9, Comparative Examples 1-10)
Examples 2 to 9 and Comparative Examples 1 to 10 were evaluated in the same manner as in Example 1 except that the scouring dyeing assistant of Example 1 was changed to the scouring dyeing assistants of the components shown in Tables 1 and 2. . The results are shown in Table 3.

  From Table 3, it can be seen that the production method of the polyester dyed fiber of the present invention and the scouring dyeing assistant of the present invention exhibit excellent scouring properties, dyeability and anti-spec specifications.

(Example 1B)
The scouring property and dyeability of the polyester dyed fiber were evaluated in the same manner as in Example 1, except that the scouring dyeing bath of Example 1 was changed to the following scouring dyeing bath containing a flame retardant and a light resistance agent. The results are shown in Table 4.

-Scouring dyeing bath The scouring dyeing assistant of Example 1 was introduced to a concentration of 1 g / L in a mini-color dedicated dyeing pot charged with water, and then Kaylon Polyester Black RV-SF300 (3 wt% owf). , Manufactured by Nippon Kayaku Co., Ltd.) while being dissolved in water at 30 to 35 ° C., followed by Flamguard CP-3 (10% by weight owf, aqueous dispersion, Matsumoto Yushi Seiyaku ( Brian FOK-3 (2% by weight owf, aqueous dispersion, manufactured by Matsumoto Yushi Seiyaku Co., Ltd.) was added and stirred as a drug containing a light-resistant agent. Thereafter, the pH was adjusted to 4.5 with an acetic acid / sodium acetate buffer to prepare a scouring dyeing bath.

<Dispersibility of flame retardant and light proofing agent>
Regarding the dispersibility of the flame retardant and light proofing agent, the scouring dyeing bath was changed to the following scouring dyeing bath containing the flame retardant and / or light proofing agent in the anti-spec specifications of Example 1, and the evaluation criteria were as follows. Except for the above, the same evaluation method was used. The results are shown in Table 4.
If the dispersibility of the flame retardant and light proofing agent is poor, it is considered that not only a large amount of stains in the dyeing machine will be generated, but also the flame retardancy or light resistance of the dyed product will be reduced.

-Scouring dyeing bath The scouring dyeing assistant of Example 1 was introduced to a concentration of 1 g / L in a mini-color dedicated dyeing pot charged with water, and then Kaylon Polyester Black RV-SF300 (3 wt% owf). , Nippon Kayaku Co., Ltd.) was added while being dissolved in water at 30 to 35 ° C., and then any of the following (a) to (c) was added and stirred. Thereafter, the pH was adjusted to 4.5 with an acetic acid / sodium acetate buffer to prepare a scouring dyeing bath.
(A) Agent containing flame retardant: Flamguard CP-3 (10% by weight owf, aqueous dispersion, manufactured by Matsumoto Yushi Seiyaku Co., Ltd.)
(B) Agent containing light-proofing agent: Brian FOK-3 (2% by weight owf, aqueous dispersion, manufactured by Matsumoto Yushi Seiyaku Co., Ltd.)
(C) Agent containing flame retardant and agent containing light-resistant agent: Flamguard CP-3 (10% by weight owf, aqueous dispersion, manufactured by Matsumoto Yushi Seiyaku Co., Ltd.) and Brian FOK-3 (2% by weight owf, Water dispersion, manufactured by Matsumoto Yushi Seiyaku Co., Ltd.)

-Evaluation criteria for dispersibility of flame retardant and light-proofing agent Evaluation was performed according to the following criteria with the filter paper naturally dried.
○: Almost no color on filter paper.
X: Specs or aggregates are present on the entire surface of the filter paper (the same level as when filtering a scoured dyeing solution obtained by treating a blank (BL, Comparative Example 7B) not containing a scouring dyeing assistant with a mini color).
Δ: Specs or aggregates are present on the entire surface of the filter paper (intermediate level between ○ and ×).

(Examples 2B to 9B, Comparative Examples 1B to 10B)
Examples 2B to 9B and Comparative Examples 1B to 10B are the same as Example 1B, except that the scouring dyeing assistant of Example 1 is changed to the scouring dyeing assistants of Examples 2 to 10 and Comparative Examples 1 to 10, respectively. And evaluated. The results are shown in Table 4.

  From Table 4, it can be seen that the production method of the polyester-based dyed fiber of the present invention and the scouring dyeing assistant of the present invention exhibit excellent dispersibility of the flame retardant / lightproofing agent in addition to excellent scouring property and dyeability.

  In the method for producing a polyester dyed fiber of the present invention, a scouring and dyeing process can be performed in one bath, and a polyester dyed fiber having good scouring properties and dyeing properties can be obtained. The scouring and dyeing assistant of the present invention is used for scouring and dyeing in one bath, and exhibits the same effect.

Claims (11)

A process for producing a polyester-based dyed fiber in which scouring and dyeing of raw material polyester fiber is performed in one bath,
A method for producing a polyester dyed fiber, wherein the bath contains a nonionic surfactant (A) represented by the following general formula (1), an anionic surfactant (B) represented by the following general formula (2), and a disperse dye. .

(In the formula, A ¹ O is an oxyethylene group or an oxypropylene group, and may be one or two types. N is an integer of 2 to 50, and p is 1 or 2.)

(In the formula, A ² O is an oxyethylene group or an oxypropylene group, and may be one or two types. M is an integer of 2 to 50, q is 1 or 2, and M is Hydrogen atom, alkali metal, alkaline earth metal, ammonium, quaternary ammonium, alkylamine or alkanolamine.)   The method for producing a polyester-based dyed fiber according to claim 1, wherein the treatment is performed under acidic conditions.   The manufacturing method of the polyester dyeing fiber of Claim 1 or 2 whose pH (25 degreeC) of the said bath is 3-6.   The weight ratio (A / B) of the nonionic surfactant (A) and the anionic surfactant (B) in the bath is 95/5 to 20/80. The manufacturing method of the polyester dyeing fiber of description.   The concentration of the nonionic surfactant (A) in the bath is 0.01 to 80 g / L, and the concentration of the anionic surfactant (B) in the bath is 0.01 to 70 g / L. The manufacturing method of the polyester dyeing fiber in any one of Claims 1-4.   The manufacturing method of the polyester dyeing fiber in any one of Claims 1-5 whose temperature at the time of performing the said process is 80-180 degreeC.   The method for producing a polyester-based dyed fiber according to any one of claims 1 to 6, wherein the bath further contains a flame retardant, and in addition to the treatment, the treatment for flame retardant processing is further performed in one bath.   The method for producing a polyester-based dyed fiber according to any one of claims 1 to 7, wherein the bath further contains a light-resistant agent, and in addition to the treatment, the light-resistant processing is further performed in one bath. Contains a nonionic surfactant (A) represented by the following general formula (1) and an anionic surfactant (B) represented by the following general formula (2), and is used for scouring and dyeing in one bath. , Scouring dyeing aid for polyester fiber.

(In the formula, A ¹ O is an oxyethylene group or an oxypropylene group, and may be one or two types. N is an integer of 2 to 50, and p is 1 or 2.)

(In the formula, A ² O is an oxyethylene group or an oxypropylene group, and may be one or two types. M is an integer of 2 to 50, q is 1 or 2, and M is Hydrogen atom, alkali metal, alkaline earth metal, ammonium, quaternary ammonium, alkylamine or alkanolamine.)   The scouring dyeing assistant for polyester fiber according to claim 9, wherein a weight ratio (A / B) of the nonionic surfactant (A) to the anionic surfactant (B) is 95/5 to 20/80. Agent.   The weight ratio of the nonionic surfactant (A) in the nonvolatile content of the scouring dyeing assistant is 20 to 95% by weight, and the weight ratio of the anionic surfactant (B) is 5 to 80% by weight. The polyester fiber scouring dyeing assistant according to claim 9 or 10.