CN103025953B - Production method for dyed fibers and agent for preventing undyed regions - Google Patents

Production method for dyed fibers and agent for preventing undyed regions Download PDF

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Publication number
CN103025953B
CN103025953B CN201180032587.9A CN201180032587A CN103025953B CN 103025953 B CN103025953 B CN 103025953B CN 201180032587 A CN201180032587 A CN 201180032587A CN 103025953 B CN103025953 B CN 103025953B
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fiber
carbon number
weight
ester
coloured fibre
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CN103025953A (en
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竹内准
土手裕幸
勘藤芳弘
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Matsumoto Yushi Seiyaku Co Ltd
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Matsumoto Yushi Seiyaku Co Ltd
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/36—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using mordant dyes ; using metallisable dyes
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/22—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using vat dyestuffs including indigo
    • D06P1/26—Phthalocyanine dyes
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/39—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using acid dyes
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/62—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds with sulfate, sulfonate, sulfenic or sulfinic groups
    • D06P1/621—Compounds without nitrogen
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/667—Organo-phosphorus compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/02—Material containing basic nitrogen
    • D06P3/04—Material containing basic nitrogen containing amide groups
    • D06P3/24—Polyamides; Polyurethanes
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/02—Material containing basic nitrogen
    • D06P3/04—Material containing basic nitrogen containing amide groups
    • D06P3/24—Polyamides; Polyurethanes
    • D06P3/241—Polyamides; Polyurethanes using acid dyes
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/02—Material containing basic nitrogen
    • D06P3/04—Material containing basic nitrogen containing amide groups
    • D06P3/24—Polyamides; Polyurethanes
    • D06P3/245—Polyamides; Polyurethanes using metallisable or mordant dyes

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Coloring (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Artificial Filaments (AREA)

Abstract

The purpose of the present invention is to provide an efficient production method for dyed fibers that reduces undyed regions when dying raw material fiber containing a silicon component and to provide an agent for preventing undyed regions, that can be suitably used in said method. The production method for dyed fiber includes a step for dying the raw material fiber that contains a silicon component, in a dye bath that includes a dye and at least one kind of ester selected from a phosphoric acid ester (A) indicated by general formula (1) and a sulfate ester (B) indicated by general formula (2).

Description

The manufacture method of coloured fibre and prevent not stain
Technical field
The present invention relates to the manufacture method of coloured fibre and prevent not stain.
Background technology
In recent years, at the filature of fiber, weave etc. in various operations, use the preparation that contains silicone composition.Silicone composition has high lipophile conventionally, makes dyestuff caking in the dyeing process that has used water-soluble dye, hinders fixing of dye, is unstained.For this reason, in the situation that the raw fiber that contains silicone composition is dyeed with general water-soluble dye, before dyeing, in order to remove silicone composition from raw fiber, need refining procedure etc.But by carrying out refining procedure, the cost of inevitable coloured fibre rises, and is disadvantageous economically, so even if the raw fiber that contains silicone composition also wishes to carry out refining procedure before dyeing process.But, in reality, have due to undyed problem, being difficult to omit refining procedure is present situation.
As the typical example of the fiber that contains silicone composition, for example, there is the composite fibre by polyamide fiber coating with elastomeric polyurethane fiber.As polyurethane fiber, conventionally, in the spinning process for the manufacture of it, in order to improve draftability, flatness and easy zbility, prevent embrittlement, use the spinning oil that contains a large amount of silicone compositions.For this reason, contained silicone composition in polyurethane fiber, slowly outwards spills, and is attached to the polyamide fiber of coating polyurethane fiber, becomes the above-mentioned composite fibre that contains silicone composition.
About this composite fibre, if carried out refining procedure before dyeing process, be disadvantageous economically, but can avoid undyed problem.For example, in patent documentation 1, the stage before the fibrous material that contains polyurethane fiber material is carried out to high-temperature heat treatment is disclosed, together with refining agent, sulfoacid compound and salt thereof are put into refining groove, except the method for degreaser composition and metal ingredient, dyeing difficulty is solved.But in the method, due to silicone composition is removed from fibrous material, so the draftability of polyurethane fiber declines greatly, the other problems of embrittlement and so on can occur.So, in the situation that the composite fibre that contains polyurethane fiber is dyeed, because of having or not of silicone composition contrary composite fibre be unstained and the problem utmost point of embrittlement is difficult to good balance and solves.
[prior art document]
[patent documentation]
Patent documentation 1: TOHKEMY 2005-42236 communique
Summary of the invention
The object of the invention is to, provide when the raw fiber that contains silicone composition is dyeed suppress to be unstained and the manufacture method of the coloured fibre that efficiency is high and can be suitably for the not stain that prevents of the method.
[for solving the means of problem]
The inventor etc. concentrate on studies in order to solve above-mentioned problem, found that so long as the method in the dye bath that contains dyestuff and specific ester, the raw fiber that contains silicone composition being dyeed, can be in the situation that not utilizing in advance refining etc. that silicone composition refining etc. is removed, can suppress to be unstained and raw fiber is dyeed, thereby having realized the present invention.
; the manufacture method of coloured fibre of the present invention; it comprises: in the dye bath of at least a kind of ester selecting the sulfuric ester (B) that contains dyestuff and the phosphate (A) representing from following general formula (1) and following general formula (2) expression, and the operation that the raw fiber that contains silicone composition is dyeed.
[changing 1]
(in formula, R 1the alkyl of carbon number 2～30, the aralkyl of the aryl of carbon number 6～30 or carbon number 7～30, A 1o is the oxyalkylene group of carbon number 2～4, and n is 0～50 integer, and m is 1～3 integer, M 1it is the group that hydrogen atom, alkali metal, alkaline-earth metal or following general formula (3) represent.)
[changing 2]
(in formula, R 2the alkyl of carbon number 2～30, the aralkyl of the aryl of carbon number 6～30 or carbon number 7～30, A 2o is the oxyalkylene group of carbon number 2～4, and l is 0～50 integer, M 2it is the group that hydrogen atom, alkali metal, alkaline-earth metal or following general formula (3) represent.)
[changing 3]
(in formula, R a, R b, R cand R dhydrogen atom, alkyl, silane alcohol base or polyoxyalkylenes, can be mutually the same, also can be different.)
In the manufacture method of this coloured fibre, preferably meet at least 1 in following (1)～(5).
(1) above-mentioned dyestuff is water miscible dyestuff.
(2) above-mentioned raw materials fiber contains polyamide fiber.
(3) above-mentioned raw materials fiber contains polyurethane fiber.
(4), with respect to above-mentioned raw materials fabric integer, the containing ratio of above-mentioned silicone composition is more than 0.01 % by weight.
(5) 0.001～50 % by weight that the concentration of above-mentioned ester is above-mentioned dye bath.
Coloured fibre of the present invention is the fiber that utilizes above-mentioned manufacture method to obtain.
The not stain that prevents of the present invention is used when the raw fiber that contains silicone composition is dyeed, and contains at least a kind of ester selecting from above-mentioned phosphate (A) and above-mentioned sulfuric ester (B).
[effect of invention]
In the manufacture method of coloured fibre of the present invention, when being dyeed, suppresses the raw fiber that contains silicone composition to be unstained, can obtain efficiently coloured fibre.In addition, in this manufacture method, the situation that raw fiber contains polyurethane fiber (situation that particularly contains polyamide fiber and polyurethane fiber), cannot solve above-mentioned being unstained and the problem of embrittlement with good balance in the past, even if can not dye but do not carry out refining yet, the embrittlement that the draftability that does not produce polyurethane fiber declines and so on greatly.
The not stain that prevents of the present invention, can perform well in above-mentioned manufacture method.
The specific embodiment
The manufacture method of coloured fibre of the present invention, it is the manufacture method that comprises following operation, that is, in the dye bath of at least a kind of ester that contains dyestuff and select from above-mentioned phosphate (A) and above-mentioned sulfuric ester (B), the operation that the raw fiber that contains silicone composition is dyeed.Coloured fibre of the present invention is the fiber that utilizes this manufacture method to obtain.The not stain that prevents of the present invention is used when the raw fiber that contains silicone composition is dyeed, and is the preparation that contains this ester.Below describe in detail.
(ester)
Ester is to be suppressed at the undyed composition that must comprise in the dye bath using in manufacture method of the present invention.About ester, even if be that have silicone composition to exist to think also can be as the composition that dye diffusion is played a role to the carrier in raw fiber.
In the situation that contains polyurethane fiber at raw fiber (situation that particularly contains polyamide fiber and polyurethane fiber), not only do not need to suppress to be unstained, do not need dyeing refining before yet.Its result, the embrittlement that the draftability that does not occur in the polyurethane fiber occurring in the situation of the refining before dyeing declines and so on greatly.
Ester is at least a kind that from phosphate (A) and sulfuric ester (B), selects.
Phosphate (A) is the phosphate that general formula (1) represents, can be any of phosphotriester, di-phosphate ester, phosphate monoester, can be their mixture.On the other hand, sulfuric ester (B) is the sulfuric acid monoester that general formula (2) represents.
In general formula (1) and (2), R 1and R 2all alkyl, 6～30 aryl or the aralkyl of carbon number 7～30 of carbon number 2～30.R 1and R 2in, the carbon a few hours of group separately, hydrophily raises, and with respect to the delivery effect decline of silicone composition, has not therefore given play to and has prevented fully not metachromia.On the other hand, when the carbon number of group is separately larger, hydrophobicity raises, and therefore the decreased solubility to water has not been given play to and prevented fully not metachromia.
The carbon number of alkyl is generally 2～30, and preferably 4～26, further preferably 6～24, particularly preferably 8～22.As such alkyl, such as enumerating octyl group, decyl, lauryl, tridecyl, isotridecyl, cetyl, stearyl, oleyl, mountain Yu base etc.
The carbon number of aryl is generally 6～30, and preferably 7～17, further preferably 8～16, particularly preferably 9～15.As such aryl, such as enumerating phenyl, biphenyl, naphthyl, anthryl, phenanthryl etc.
The carbon number of aralkyl is generally 7～30, and preferably 8～28, further preferably 9～26, particularly preferably 10～24.As such aralkyl, such as enumerating benzyl, phenylethyl, methyl-benzyl, naphthyl methyl etc.
It should be noted that, above-mentioned aryl and aralkyl can have substituting group, and substituent carbon number is generally 1～30, and preferably 2～26, further preferably 3～24.As such substituting group, can enumerate methyl, ethyl, t-butyl, octyl group, nonyl, lauryl, decyl, tridecyl, isotridecyl, cetyl, stearyl, oleyl, Shan Yu base, styryl etc.Substituent number like this can be 1, can be also a plurality of, is having a plurality of in the situation that, can be that multiple substituting group mixes and exists.
In general formula (1) and (2), A 1o and A 2o is all oxyalkylene groups of carbon number 2～4, carbon number preferably 2～3, further preferably 2.A 1o and A 2o is all a kind or two or more, in situation of more than two kinds, can form block addition product, any of addition product or random addition product alternately.From the deliquescent viewpoint water, A 1o and A 2o all preferably must contain oxyethylene group.Oxyethylene group shared ratio in whole oxyalkylene group is preferably more than 40 % by mole, more preferably 50 % by mole, more preferably more than 60 % by mole, is particularly preferably more than 80 % by mole.
In general formula (1) and (2), n and l are 0～50 integer, and preferably 1～45, further preferably 2～40, particularly preferably 3～35.When integer is excessive, for the delivery effect decline of silicone composition, can bring into play and prevent fully not metachromia.On the other hand, when integer is too small, the decreased solubility in water, does not prevent not metachromia fully so can not bring into play.
In general formula (1), m is 1～3 integer, preferably 1～2.
In general formula (1) and (2), M 1and M 2the group that hydrogen atom, alkali metal, alkaline-earth metal or above-mentioned general formula (3) represent, the group that preferred as alkali, alkaline-earth metal or above-mentioned general formula (3) represent.
As alkali metal, such as enumerating lithium, sodium, potassium etc.
As alkaline-earth metal, such as enumerating magnesium, calcium, barium etc.
In the group representing at general formula (3), R a, R b, R cand R dbe hydrogen atom, alkyl, silane alcohol base or polyoxyalkylenes, they can be mutually the same, also can be different.The carbon number of alkyl is generally 1～30, and preferably 1～10.As such alkyl, such as enumerating methyl, ethyl, n-propyl group, isopropyl etc.The carbon number of silane alcohol base is generally 1～30, and preferably 1～10.As such silane alcohol base, such as enumerating methanol-based, ethanol based, n-propyl alcohol base, isopropyl alcohol radical etc.The carbon number of polyoxyalkylenes is generally 2～60, and preferably 4～30.As such polyoxyalkylenes, such as enumerating polyoxyethylene groups, polyoxypropylene base etc.
Phosphate (A) can be manufactured by known method.As the manufacture method of phosphate (A), for example known have a phosphorylation reaction carrying out based on raw alcohol and phosphoric anhydride, then according to circumstances by neutralization, obtains the method for phosphate (A).By the input mol ratio of feed change alcohol and phosphoric anhydride, can roughly separately make diester and monoesters here.For example,, at raw alcohol: phosphoric anhydride=1: the in the situation that of 1 (mol ratio), mainly obtain monoesters (m=1 in general formula (1)).At raw alcohol: phosphoric anhydride=2: the in the situation that of 1 (mol ratio), mainly obtain diester (m=2 in general formula (1)).
Sulfuric ester (B) also can be manufactured by known method.As the manufacture method of sulfuric ester (B), have as everyone knows and for example carry out the sulfating reaction based on raw alcohol and sulfuric acid, then according to circumstances by neutralization, obtain the method for sulfuric ester (B).
(dyestuff)
Dyestuff is the composition that must be contained together with ester in the dye bath using in manufacture method of the present invention.About dyestuff, be not particularly limited, but water miscible dyestuff is because dyeing preferably to the raw fiber using in the present invention.As water miscible dyestuff, such as enumerating ACID DYES, acid mordant dyes, metal complex dyes, reactive dye, cation dyes etc.Water miscible dyestuff preferred acidic dyestuff, acid mordant dyes, metal complex dyes and reactive dye, further preferred acidic dyestuff, acid mordant dyes and metal complex dyes.
As ACID DYES, such as enumerating Kayacyl Colours dyestuff, Kayanol Colours dyestuff, Kayanol Milling Colours dyestuff, Telon dyestuff, Supranol dyestuff, NEOLAN dyestuff, Nylomine dyestuff, Suminol dyestuff etc.Acid mordant dyes, for example, Diamond dyestuff, Sunchromine dyestuff etc.As metal complex dyes, such as enumerating KayakalanColours dyestuff, Kayalax Colours dyestuff, Isolan dyestuff, Lanafast dyestuff, LANACRON dyestuff etc.
(other compositions)
In dye bath, except ester and dyestuff, must contain water.As water, can be any of pure water, distilled water, Purified Water, soft water, ion exchange water, running water etc.
In addition, dye bath can contain except other compositions it in the scope of not damaging effect of the present invention.As other compositions, such as enumerating softener, antistatic agent, defoamer, solvent, aliphatic acid (salt) etc. in anion surfactant, non-ionic surface active agent, cationic surfactant, amphoteric surfactant, pH adjusting agent, chelating agent, fixer, fire retardant, photostabilizer, slow levelling agent, bath.
As pH adjusting agent, can enumerate acetic acid, sodium acetate, lactic acid, sodium lactate, phosphoric acid, sodium dihydrogen phosphate, sodium hydrogen phosphate, tertiary sodium phosphate etc.
As chelating agent, such as enumerating polycarboxylic acids, complexon I (NTA), ethylenediamine tetra-acetic acid (EDTA), inferior amino trimethylene methyl acid phosphate, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid (NTMP), phosphoric acid, glutamic acid oxalic acid and their salt etc.
As fixer, be not particularly limited, but can enumerate natural tannin, syntannins, quaternary ammonium salt, pyridiniujm, polyamine based polymer etc.They can be used singly or in combination.Preferred natural tannin, syntannins.
Example as syntannins, such as having, to using material that phenol, cresols, benzoic acid, naphthols, bis-phenol etc. have a phenol hydroxyl be syntannins as phenolic varnish type or the first rank phenolic varnish type phenol of raw material, the benzenethiol that the phenols such as phenol, o-chlorophenol and sulphur is raw material through the condensation product that obtains of sulfuration of take is syntannins, dihydroxy-diphenyl sulfone is syntannins, naphthalene is that syntannins, sulfonamide are that syntannins, carbodiimides are syntannins etc., and they use separately respectively or are used as the mixture of arbitrary proportion etc.
As natural tannin, be condensed type tannin, water-disintegrable tannin and with the two the general name of compound tannin of character.Extensively to have the organic compound that the polyhydric phenols in trunk, bark, branch, tree root, seed, fruit, leaf etc. is basic structure.
As slow levelling agent, can use the dye leveller of known close fibroid dye leveller in the past and/or close dyestuff.
As softener in bathing, be not particularly limited, but can enumerate the ester compounds of polyoxyethylene deriv, polyamide-based polymeric derivative, lanolin epoxide, alkyl polyamine derivatives, higher fatty acids ester derivant, polyoxyethylene alkyl amine and aliphatic acid, high alcohol ester derivative of trimellitic acid, polyacrylamide derivative etc.
(raw fiber)
As long as the raw fiber using in the present invention contains silicone composition, be just not particularly limited.In addition, the raw fiber using in the present invention, can be not only the fiber dyeing, and can also be dye but in fact achromophil fiber has occurred.Now, undyed fiber has occurred and through manufacture method of the present invention, dyeed once again, coloured fibre suppressed, that eliminate can obtain being unstained.
Form about raw fiber, is not particularly limited, and can be any shapes such as silk, braided fabric, textiles, cheese, Guang line.
Kind about raw fiber, is not particularly limited, but preferably with synthetic fiber such as polyamide fiber, polyacrylic fibre, vinylon fibers; The natural fabrics such as cotton, fiber crops, wool, silk goods; The fiber that the fibers such as regenerated fiber (A) such as artificial silk, Ku Pula, acetic acid esters, Lyocell are essential component.In these fibers (A), preferred polyamide fiber.
Polyamide fiber refer to take polyamide as essential component can be by the fiber of Composite.Such as enumerating nylon 6, nylon 66, NYLON610, nylon 11, nylon 4, nylon 7, aromatic nylon (aromatic polyamides) etc.Polyamide can obtain through condensation by forming the reaction of amido link conventionally.
Raw fiber can be together with fiber (A), suitably to contain the fiber of the fibers (B) such as polyurethane fiber, polyester fiber, acid fiber by polylactic.In these fibers (B), optimization polyurethane fiber.
As polyurethane fiber, such as enumerating, make polytetramethylene glycol (PTMG), polyester-diol and organic diisocyanate reacts, then by Isosorbide-5-Nitrae-butanediol, ethylenediamine, propane diamine, pentane diamine etc., carried out fiber chain elongation, polyurethane or polyurethane-urea formation.About puu fiber, for example prepare PTMG and the methyl diphenylene diisocyanate (MDI) of molecular weight 1000～3000, with PTMG/MDI=1/2～1/1.5 (mol ratio), in dimethylacetylamide, dimethyl formamide equal solvent, make its reaction, with diamines such as ethylenediamine, propanediamine, carry out chain elongation and obtain polyurethaneurea polymer, with dry spinning, with spinning speed 400～1200m/min, 20～40% solution of polyurethaneurea polymer obtained above are carried out to spinning, can manufacture thus.The adaptation fineness of polyurethane fiber is not particularly limited.
In the situation that raw fiber contains fiber (A) and fiber (B), fiber (B) with respect to fiber (A) part by weight be preferably 1～90 % by weight, 5～70 % by weight more preferably.
Raw fiber preferably contains polyamide fiber and polyurethane fiber.
Silicone composition contained in raw fiber is not particularly limited, but such as enumerating dimethyl silscone (dimethyl silicone polymer), PSI, poly-methyl alkyl siloxane, modified silicone, silicone resin etc., can be formed by a kind or two or more.At least 1 place that modified silicone typically refers to two ends that have at polysiloxanes such as dimethyl silscones, single end, side chain, side chain terminal is combined with the material of the structure of at least one reactivity (sense) group or non-reacted (sense) group.In addition, silicone resin refers to the silicone with 3 dimension cross-linked structures.The modified silicone that can also contain other.
Containing ratio about silicone composition, is not particularly limited, but whole with respect to raw fiber, preferably more than 0.01 % by weight, further preferably more than 0.05 % by weight, particularly preferably more than 0.1 % by weight, most preferably more than 0.5 % by weight.The upper limit of the containing ratio of silicone composition is 100 % by weight preferably, further preferred 50 % by weight.
(manufacture method of coloured fibre)
The manufacture method of coloured fibre of the present invention, is included in the manufacture method of the operation in the dye bath that contains dyestuff and ester, raw fiber being dyeed.
As manufacture method of the present invention, for example the ratio with regulation carries out mix and blend to ester, dyestuff and water, adds pH adjusting agent as required and is adjusted to the pH (25 ℃) of regulation, prepares dyeing liquor (dye bath).Ester can mix with dyestuff philosophy singly, can also prevent that stain does not mix as described later.
Then, in dye bath, add raw fiber, dye bath is heated to the dyeing temperature of regulation, at this temperature, keep for example 10～90 minutes, carry out dyeing process.After dyeing process finishes, in order to wash on the coloured fibre obtaining the not dyestuff of set off, coloured fibre is implemented to hot water wash, washing or soap cleaning etc.For coloured fibre, in order to improve fastness, and then can carry out photographic fixing processing.The method of processing as photographic fixing, is not particularly limited, and can adopt known gimmick, as fixer, can use above-mentioned fixer.Then, be dried and can obtain coloured fibre.With regard to utilizing the coloured fibre that such manufacture method obtains, suppressed to be unstained.
In addition, the manufacture method of coloured fibre of the present invention comprises following operation: use and the undyed fiber that contains silicone composition has occurred as raw fiber, the operation in the dye bath that contains dyestuff and ester, this raw fiber being dyeed.That is, the manufacture method of coloured fibre of the present invention, also comprises in fact the situation that undyed fiber uses the method identical with aforesaid method to be dyeed has occurred for dyeing.And then, for more infallible, suppress to be unstained, also can repeatedly carry out same procedure.About the coloured fibre obtaining, suppressed, the elimination of being unstained.
Concentration about the ester in dye bath, is not particularly limited, but is preferably 0.001～50 % by weight of dye bath, further preferred 0.01～30 % by weight, particularly preferably 0.1～10%.In the situation that the concentration of ester, lower than 0.001%, is understood the not shown inhibition of being unstained fully.On the other hand, in the situation that the concentration of ester surpasses 50%, economically can be not preferred.
Concentration about dyestuff, is not particularly limited, but with respect to raw fiber, is preferably 0.01～50 % by weight owf (on weight of fiber), further preferably 0.1～40 % by weight owf, particularly preferably 0.2～30 % by weight owf.
As the manufacture method of coloured fibre, for example, enumerate following.First, ester, dyestuff and water are put in dyeing machine and carried out mix and blend, then add pH adjusting agent, pH is adjusted to 3.0～7.0, prepare dyeing liquor (dye bath).Then, raw fiber is put in the dyeing machine that is full of dye bath, limit makes dye bath convection current, and limit is heated to 70～110 ℃ with 1 minute ratio of 0.5～3.0 ℃ by the temperature of dye bath.Reach after this temperature, limit keeps this temperature to make dye bath convection current, and limit keeps 10～90 minutes.Then, cooling, 30～80 ℃ of drainings, feedwater again, hot water wash, the washing carried out 1～10 minute are processed.After draining, make coloured fibre dry, for coloured fibre, can not occur in undyed situation, dyeing to be finished.
In the manufacture method of coloured fibre of the present invention, in advance raw fiber is carried out to refining procedure etc., can not remove silicone composition, can be omitted in the refining procedure that carries out before dyeing process etc. for removing the operation of silicone composition.
The coloured fibre obtaining in manufacture method of the present invention, can suppress to be unstained, and is roughly dyeed equably.
In addition, in the situation that raw fiber contains polyurethane fiber, the coloured fibre obtaining in manufacture method of the present invention, is not only unstained and is suppressed, and the embrittlement that greatly declines and so on of the draftability that fiber do not occur.
Containing ratio about the silicone composition of coloured fibre of the present invention is whole with respect to coloured fibre, preferably more than 0.01 % by weight, further preferably more than 0.05 % by weight, particularly preferably more than 0.1 % by weight, most preferably more than 0.5 % by weight.The upper limit of the containing ratio of silicone composition is 100 % by weight preferably, further preferred 50 % by weight.
With respect to the rate of change (the silicone containing ratio of the silicone containing ratio/raw fiber of coloured fibre) of the silicone composition of the coloured fibre of raw fiber, from preventing the viewpoint of embrittlement, preferably more than 0.6, more preferably more than 0.7, further preferably more than 0.8.
(preventing not stain)
The not stain that prevents of the present invention is the preparation using when the raw fiber that contains silicone composition is dyeed.This prevents the ester that stain does not contain above-mentioned middle explanation, is suitable for the manufacture method of above-mentioned middle explanation.In raw fiber, not only contain the fiber dyeing, also contain and dye but undyed fiber has occurred reality.
About preventing not stain, except ester, also contain other compositions of water, above-mentioned middle explanation.Ester shared part by weight in preventing not stain is preferably 1～100 % by weight, more preferably 3～95 % by weight, more preferably 5～90 % by weight.
As the method that prevents that stain is not manufactured of the present invention, be not particularly limited, can adopt known gimmick.Such as enumerating, formation is prevented to each composition of stain is not put into method being uniformly mixed in water etc.
[embodiment]
Below, embodiments of the invention are shown, further describe the present invention, but the present invention are not limited by these embodiment.It should be noted that, " part " in example and " % " represent respectively " weight portion " and " % by weight ".
(embodiment 1)
(preventing not stain)
To possessing in the reaction vessel of 3 liters of capacity of thermometer and mixer, add polyoxyethylene (5mol) three decyl ethers (three decyl ethers that the addition molal quantity of oxygen ethene the is 5) 709g as raw alcohol, the reaction temperature with 40～60 ℃ under nitrogen atmosphere slowly drops into phosphoric anhydride 85g.80 ℃ of reactions of carrying out 3 hours, obtained yellow product.In the product obtaining, add diethanol amine 206g, carry out neutralization reaction, obtained phosphate.
To adding water in the phosphate obtaining and obtain containing the not stain that prevents of phosphate.What obtain prevents ester and the water that stain does not contain the structure shown in table 1, and ester shared part by weight in preventing not stain is 20 % by weight.
(coloured fibre)
Preparation is by the composite fibre (mass ratio 80/20: braided fabric) containing ratio of formation and silicone composition is the raw fiber of 2.20 % by weight of integral body of polyamide fiber (6-nylon) and polyurethane fiber.
By what obtain in above-mentioned, prevent that stain is not put into Mini Color special dyeing tank (TEXAM skill is ground (strain) company system), after the Kayanol Milling Turquoise 3G as dyestuff (Japanese chemical drug (strain) company system) is dissolved in the water of 30～35 ℃, add.Finally, with acetic acid/sodium acetate buffer, be adjusted to pH4.5, prepared dye bath.Here, the concentration of ester is 2.0 % by weight of dye bath, and the concentration of dyestuff is to be 2.0 % by weight owf with respect to raw fiber.
Raw fiber is put in dye bath, with Mini Color, processed.(the raw fiber weight: dye bath weight) be 1: 10 of bath raio now.Dyeing treatment conditions are, with the programming rate of 2 ℃/min, dye bath is heated to 95 ℃, and 95 ℃ are kept 60 minutes.Then, cooling while making it reach 80 ℃, discarded dye bath, carries out hot water wash, the washing of 1 minute.Then, utilize centrifugal separating device to dewater to the fiber obtaining, at 90 ℃, be dried 1 hour, obtained coloured fibre.Utilize following method to coloured fibre do not dye preventive and embrittlement degree is evaluated.The results are shown in table 1.
< does not dye preventive >
By following benchmark, the preventive of not dying of coloured fibre is carried out to visual valuation.
◎: completely have no and be unstained on coloured fibre, can dye equably.
Zero: on coloured fibre, be slightly unstained as seen, can roughly dye equably.
*: clearly visible being unstained on coloured fibre, cannot dye equably.
< embrittlement degree >
With JIS-L-1018 constantly acting load method, the percentage elongation of coloured fibre is measured, evaluated the embrittlement degree of fiber.Mensuration is to use Compression and Expansion testing machine Technograph TG-2KN (Minebea (strain) company system) to carry out in the measuring cell that keeps 20 ℃ of temperature and humidity 65%RH.From coloured fibre, cut out test cloth sheet (length 10cm, width 2cm), apply constantly acting load (15N) watt strangling direction, coloured fibre is stretched, measured percentage elongation.It should be noted that, the percentage elongation of comparative example 1 (blank) of take is benchmark, utilizes following method to evaluate the embrittlement degree of coloured fibre.
Zero: the percentage elongation of coloured fibre is the more than 90% of percentage elongation of comparative example 1
△: the percentage elongation of coloured fibre surpass comparative example 1 percentage elongation 70% and lower than 90%
*: the percentage elongation of coloured fibre is below 70% of percentage elongation of comparative example 1
(embodiment 2～5)
In embodiment 1, in change raw fiber as shown in table 1, the contained containing ratio of silicone composition and the concentration of ester, manufactured respectively in the same manner as in Example 1 coloured fibre, and evaluated.Its result is also shown in table 1.
(embodiment 6～16)
Carry out in the same manner as in Example 1 the phosphorylation reaction based on raw alcohol and phosphoric anhydride, manufactured respectively the not stain that prevents that contains the ester shown in table 1.It should be noted that, the oxyalkylene group of the raw alcohol in embodiment 15,16 is random addition.
In embodiment 1, except the kind of the ester that change is used as shown in table 1 respectively, use and prevent not stain in the same manner as in Example 1, manufactured respectively coloured fibre, and evaluated.Its result is also shown in table 1.
(embodiment 17)
(preventing not stain)
To having in the reaction vessel of 3 liters of capacity of thermometer and mixer, add polyoxyethylene (18mol) stearyl ether (stearyl ether that the addition molal quantity of oxygen ethene the is 18) 825g as raw alcohol, the reaction temperature with 40～60 ℃ under nitrogen atmosphere slowly packs sulfuric acid (98 % by weight) 85g into.70 ℃ of reactions of carrying out 3 hours, obtained white product.In the product obtaining, add diethanol amine 90g, carry out neutralization reaction, obtained sulfuric ester.
To adding water in the sulfuric ester obtaining and obtain containing the not stain that prevents of sulfuric ester.What obtain prevents ester and the water that stain does not contain the structure shown in table 2, and ester shared part by weight in preventing not stain is 20 % by weight.
(coloured fibre)
By what use in embodiment 1, prevent that stain does not change to the not stain that prevents obtaining here, in addition manufactured in the same manner as in Example 1 coloured fibre, and evaluated.Its result is also shown in table 2.
(embodiment 18～27)
The sulfating reaction that carry out based on raw alcohol and sulfuric acid the same as embodiment 17, has manufactured respectively the not stain that prevents that contains the ester shown in table 2.
In embodiment 17, except the kind of the ester that uses of change respectively as shown in table 2, equally with embodiment 17 manufactured respectively coloured fibre, and evaluated.Its result is also shown in table 2.
(embodiment 28)
By the not stain that prevents using in embodiment 1, change to mix embodiment 1 prevent stain not and embodiment 17 prevent stain not and the mixing that obtains prevents (contained ester weight portion=50 in stain that prevent not that prevent contained ester weight portion: embodiment 17 in stain not of embodiment 1: 50) of stain not, in addition manufactured in the same manner as in Example 1 coloured fibre, and evaluated.Its result is also shown in table 2.
(embodiment 29)
By the not stain that prevents using in embodiment 1, change to mix embodiment 1 prevent stain not and embodiment 17 prevent stain not and the mixing that obtains prevents (contained ester weight portion=70 in stain that prevent not that prevent contained ester weight portion: embodiment 17 in stain not of embodiment 1: 30) of stain not, in addition manufactured in the same manner as in Example 1 coloured fibre, and evaluated.Its result is also shown in table 2.
(comparative example 1)
In embodiment 1, except not using, prevent from not stain, having manufactured in the same manner as in Example 1 coloured fibre, and having evaluated.The results are shown in table 3.
(comparative example 2～9)
In embodiment 1, the compound shown in use table 3 replaces preventing not stain respectively, and making its concentration is 2.0 % by weight of dye bath, in addition, has manufactured respectively in the same manner as in Example 1 coloured fibre, and has evaluated.The results are shown in table 3.
[table 1]
[table 2]
[table 3]
From table 1～3, with of the present invention, prevent that stain is not manufactured coloured fibre in the situation that, the excellent preventive of not dying is being shown.
(embodiment 1b～29b, comparative example 1b～9b)
In embodiment 1b～29b and comparative example 1b～9b, the generation of manufacturing in using comparative example 1 undyed coloured fibre as raw fiber, with each embodiment, the same coloured fibre of having manufactured respectively embodiment 1b～29b and comparative example 1b～9b of comparative example.That has evaluated respectively the coloured fibre that obtains does not dye preventive, embrittlement degree.The results are shown in table 4,5.
[table 4],
[table 5]
From table 4,5, by manufacture method of the present invention and prevent not stain, even if in the situation that use has occurred undyed coloured fibre as raw fiber, the excellent preventive of not dying is also shown.
(comparative example 10)
The mode that is refining agent SSK-4 (pine this grease pharmacy (strain) company system) 1.0 % by weight and soda ash 0.2 % by weight according to the concentration of bathing with respect to refining is prepared refining and is bathed, and with the raw fiber that refining is bathed using in embodiment 1, processes.Bath raio now (raw fiber weight: weight is bathed in refining) is 1: 10.Refining treatment condition is with the programming rate of 2 ℃/min, refining to be bathed and is heated to 80 ℃, and 80 ℃ are kept 60 minutes.Then, cooling while making it reach 60 ℃, discarded refining is bathed, and carries out hot water wash, the washing of 1 minute.Then, utilize centrifugal separating device to dewater to the fiber obtaining, at 90 ℃, be dried 1 hour, obtained refining fiber.
The raw fiber using in embodiment 1 is changed to above-mentioned refining fiber, and do not use and prevent not stain, in addition, manufactured in the same manner as in Example 1 coloured fibre, and evaluated.That does not dye preventive is evaluated as zero, being evaluated as of embrittlement degree * and, the remarkable hardening of coloured fibre.
Its result, there is no need the refining procedure before dyeing, and can simplify dyeing processing.
(embodiment 30)
Prepared the composite fibre (mass ratio 90/10: textiles) containing ratio of formation and silicone composition is the raw fiber of 2.20 whole % by weight by cotton fiber and polyurethane fiber.By what obtain in embodiment 1, prevent that stain is not put in Mini Color special dyeing tank, after the Kayacion Turquoise P-3GF as dyestuff (Japanese chemical drug (strain) company system) is dissolved in the water of 30～35 ℃, add.Finally, add thenardite and soda ash, prepared dye bath.Here, the concentration of ester, thenardite and soda ash, is respectively 2.0 % by weight, 6.0 % by weight and 2.0 % by weight of dye bath, and the concentration of dyestuff is to be 2.0 % by weight owf with respect to raw fiber.
Raw fiber is put in dye bath, with Mini Color, processed.(the raw fiber weight: dye bath weight) be 1: 10 of bath raio now.Dyeing treatment conditions are, with the programming rate of 2 ℃/min, dye bath is heated to 80 ℃, and 80 ℃ are kept 60 minutes.Then, cooling while making it reach 60 ℃, discarded dye bath, carries out hot water wash, the washing of 10 minutes.Then, utilize centrifugal separating device to dewater to the fiber obtaining, at 90 ℃, be dried 1 hour, obtained coloured fibre.The coloured fibre obtaining do not dye preventive be evaluated as zero.
(embodiment 31)
The containing ratio of having prepared by wool fibre (textiles) formation and silicone composition is the raw fiber of 2.20 % by weight of integral body.By what obtain in embodiment 1, prevent that stain is not put in Mini Color special dyeing tank, after the Kayalax Colours Navy R as dyestuff (Japanese chemical drug (strain) company system) is dissolved in the water of 30～35 ℃, add.Finally, with acetic acid, be adjusted to pH5.0, prepared dye bath.Here, 2.0 % by weight that the concentration of ester is dye bath, the concentration of dyestuff is to be 2.0 % by weight owf with respect to raw fiber.
Raw fiber is put in dye bath, with Mini Color, processed.(the raw fiber weight: dye bath weight) be 1: 10 of bath raio now.Dyeing treatment conditions are, with the programming rate of 1 ℃/min, dye bath is heated to 100 ℃, and 100 ℃ are kept 45 minutes.Then, cooling while making it reach 80 ℃, discarded dye bath, carries out hot water wash, the washing of 5 minutes.Then, utilize centrifugal separating device to dewater to the fiber obtaining, at 90 ℃, be dried 1 hour, obtained coloured fibre.The coloured fibre obtaining do not dye preventive be evaluated as zero.
[utilizing possibility] in industry
The manufacture method of coloured fibre of the present invention can suitably be used when the raw fiber that contains silicone composition is dyeed.

Claims (12)

1. a manufacture method for coloured fibre, it comprises:
The operation in the dye bath of at least a kind of ester selecting the sulfuric ester (B) that contains water miscible dyestuff and the phosphate (A) representing from following general formula (1) and following general formula (2) expression, the raw fiber that contains silicone composition being dyeed,
In formula (1), R 1the alkyl of carbon number 2～30, the aralkyl of the aryl of carbon number 6～30 or carbon number 7～30, A 1o is the oxyalkylene group of carbon number 2～4, and n is 0～50 integer, and m is 1～3 integer, M 1the group that hydrogen atom, alkali metal, alkaline-earth metal or following general formula (3) represent,
In formula (2), R 2the alkyl of carbon number 2～30, the aralkyl of the aryl of carbon number 6～30 or carbon number 7～30, A 2o is the oxyalkylene group of carbon number 2～4, and l is 0～50 integer, M 2the group that hydrogen atom, alkali metal, alkaline-earth metal or following general formula (3) represent,
In formula (3), R a, R b, R cand R dhydrogen atom, alkyl, silane alcohol base or polyoxyalkylenes, can be mutually the same, also can be different.
2. the manufacture method of coloured fibre as claimed in claim 1, wherein,
Described raw fiber contains polyamide fiber.
3. the manufacture method of the coloured fibre as described in claim 1 or 2, wherein,
Described raw fiber contains polyurethane fiber.
4. the manufacture method of the coloured fibre as described in claim 1 or 2, wherein,
Whole with respect to described raw fiber, the containing ratio of described silicone composition is more than 0.01 % by weight.
5. the manufacture method of coloured fibre as claimed in claim 3, wherein,
Whole with respect to described raw fiber, the containing ratio of described silicone composition is more than 0.01 % by weight.
6. the manufacture method of the coloured fibre as described in claim 1 or 2, wherein,
The concentration of described ester is 0.001～50 % by weight of described dye bath.
7. a coloured fibre, it is obtained by the manufacture method described in any one in claim 1～6.
8. prevent a not stain, it uses when the raw fiber that contains silicone composition is dyeed,
Contain at least a kind of ester selecting the sulfuric ester (B) representing from phosphate (A) and the following general formula (2) of following general formula (1) expression,
In formula, R 1the alkyl of carbon number 2～30, the aralkyl of the aryl of carbon number 6～30 or carbon number 7～30, A 1o is the oxyalkylene group of carbon number 2～4, and n is 0～50 integer, and m is 1～3 integer, M 1the group that hydrogen atom, alkali metal, alkaline-earth metal or following general formula (3) represent,
In formula, R 2the alkyl of carbon number 2～30, the aralkyl of the aryl of carbon number 6～30 or carbon number 7～30, A 2o is the oxyalkylene group of carbon number 2～4, and l is 0～50 integer, M 2the group that hydrogen atom, alkali metal, alkaline-earth metal or following general formula (3) represent,
In formula, R a, R b, R cand R dhydrogen atom, alkyl, silane alcohol base or polyoxyalkylenes, can be mutually the same, also can be different.
9. the not stain that prevents as claimed in claim 8, wherein,
Described raw fiber contains polyamide fiber.
10. as described in claim 8 or 9, prevent not stain, wherein,
Described raw fiber contains polyurethane fiber.
11. prevent not stain as described in claim 8 or 9, wherein,
Whole with respect to described raw fiber, the containing ratio of described silicone composition is more than 0.01 % by weight.
The 12. not stains that prevent as claimed in claim 10, wherein,
Whole with respect to described raw fiber, the containing ratio of described silicone composition is more than 0.01 % by weight.
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Citations (1)

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JPS591784A (en) * 1982-06-24 1984-01-07 東邦化学工業株式会社 Dyeing aid for polyester fiber or polyester/cellulose fiber blended mixture
JPH0241479A (en) * 1988-07-27 1990-02-09 Dai Ichi Kogyo Seiyaku Co Ltd One-dip scouring dyeing aid for cellulose fiber and semisynthetic fiber
JPH06341032A (en) * 1993-05-26 1994-12-13 Toray Ind Inc Coating-processed fabric
DE10028224A1 (en) * 2000-06-07 2002-01-03 Bayer Ag Mixtures of sulfuric acid esters
JP5070852B2 (en) * 2007-01-19 2012-11-14 東レ株式会社 Manufacturing method of sheet-like material

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Publication number Priority date Publication date Assignee Title
CN1324362A (en) * 1998-10-23 2001-11-28 拜尔公司 Phosphoric acid esters

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Title
JP平2-41479A 1990.02.09
JP特开2008-174868A 2008.07.31

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