CN105189856B - Synthetic fibers inorganic agent and application thereof - Google Patents
Synthetic fibers inorganic agent and application thereof Download PDFInfo
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- CN105189856B CN105189856B CN201480019828.XA CN201480019828A CN105189856B CN 105189856 B CN105189856 B CN 105189856B CN 201480019828 A CN201480019828 A CN 201480019828A CN 105189856 B CN105189856 B CN 105189856B
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- inorganic agent
- synthetic fibers
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- polyoxyalkylene alkyl
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
- D02G1/02—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist
- D02G1/0206—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist by false-twisting
- D02G1/026—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist by false-twisting in the presence of a crimp finish
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/165—Ethers
- D06M13/17—Polyoxyalkyleneglycol ethers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/40—Reduced friction resistance, lubricant properties; Sizing compositions
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
It is an object of the invention to provide a kind of synthetic fibers inorganic agent, the product stability when low temperature of the synthetic fibers inorganic agent is taken care of is excellent, and the stability of emulsion of inorganic agent is excellent.The present invention is the synthetic fibers inorganic agent containing following polyoxyalkylene alkyl ethers represented by formula (1) etc..RO‑(EO)a‑[(PO)b/(EO)c]‑(EO)d(wherein, R represents the alkyl or alkenyl of carbon number 1~30 to H (1), can be made up of any structure of straight or branched.PO is oxygen propylidene, and EO is oxygen ethylidene.A, b, c and d represent each average addition molal quantity, a=1~10, b=1~10, c=1~10, d=1~40.[(PO)b/(EO)c]) be b moles of PO and polyoxy alkylidene obtained from c moles of the random additions of EO).
Description
Technical field
The present invention relates to synthetic fibers inorganic agent and application thereof.In more detail, product when being related to low temperature to take care of is steady
The excellent synthetic fibers inorganic agent of qualitative excellent and inorganic agent stability of emulsion (emulsion stability), use
The synthetic fiber filament yarn line and the manufacture method of false twist processing yarn of the synthetic fibers inorganic agent.
Background technology
In recent years, the production base of synthetic fibers expands, and the life of synthetic fibers is carried out in various countries, area
Produce.Thereupon, the use condition of synthetic fibers inorganic agent is directed to many-side, for example, want in temperature range wide
Inside use.
Generally, synthetic fibre treating agent is configured to flat with polyoxyalkylene alkyl ether, polyether compound, ester compounds etc.
Lubrication prescription is main body.
Now, for the PO/EO copolymers of polyoxyalkylene alkyl ether such as random type that use in the prior art or
The PO/EO copolymers of person's block type, such as inorganic agent described in patent document 1, the stability of inorganic agent, the breast of inorganic agent
Liquid stability is insufficient.
If the stability of inorganic agent is poor, with the change in storage condition (for example, winter of low temperature), composition may
Can separate.If it is fine such inorganic agent i.e. composition is there occurs that the inorganic agent of the state of separation is attached to synthesis
Dimension, then inorganic agent cannot uniformly be attached to synthetic fibers, therefore as the multiple original of the problem in yarn operation processed, manufacturing procedure
Cause.Equally, during the stability of emulsion difference of inorganic agent, inorganic agent cannot uniformly be attached to synthetic fibers, therefore as yarn operation processed
Or in manufacturing procedure the reason for problem is multiple.It should be noted that the problem of yarn operation processed mentioned here or manufacturing procedure is
Refer to, burr, broken yarn, white powder, stain of synthetic fibers etc., are the major issues of the quality of left and right synthetic fibers.
Citation
Patent document
Patent document 1：Japanese Unexamined Patent Publication 7-252774 publications
The content of the invention
The invention technical problem to be solved
It is an object of the invention to provide a kind of synthetic fibers inorganic agent, the synthetic fibers inorganic agent is when low temperature is taken care of
Product stability it is excellent, and the stability of emulsion of inorganic agent is excellent.Additionally, also provide having used the synthetic fibers to process
The synthetic fiber filament yarn line of agent, the manufacture method of synthetic fibers.
For the technological means of solve problem
The present inventor is repeated further investigation, as a result finds, if containing from the polyoxy represented by following formulas (1)
Alkylidene alkyl ether and at least one synthetic fibers by being selected in the polyoxyalkylene alkyl ether ester of following formulas (2) expression
With inorganic agent, then above-mentioned problem is can solve the problem that, so far complete the present invention.
RO-(EO)a-[(PO)b/(EO)c]-(EO)d-H (1)
(wherein, in formula (1), R represents the alkyl or alkenyl of carbon number 1~30, can be by any knot of straight or branched
Structure is constituted.PO is oxygen propylidene, and EO is oxygen ethylidene.A, b, c and d represent each average addition molal quantity, a=1~10, b=1
~10, c=1~10, d=1~40.[(PO)b/(EO)c]) polyoxy that is obtained with c moles of random additions of EO for b moles of PO
Alkylidene.)
R1O-(EO)e-[(PO)f/(EO)g]-(EO)h-CO-R2 (2)
(wherein, in formula (2), R1The alkyl or alkenyl of carbon number 1~30 is represented, can be by any of straight or branched
Structure is constituted.R2The alkyl or alkenyl of carbon number 1~30 is represented, can be made up of any structure of straight or branched.PO is
Oxygen propylidene, EO is oxygen ethylidene.E, f, g and h represent each average addition molal quantity, e=1~10, f=1~10, g=1~
10, h=1~40.[(PO)f/(EO)g] it is f moles of PO and polyoxy alkylidene obtained from g moles of the random additions of EO.)
Preferably, the fusing point of above-mentioned polyoxyalkylene alkyl ether is less than 15 DEG C.
Preferably, the cloud point of the aqueous solution of 1 weight % of above-mentioned polyoxyalkylene alkyl ether be more than 60 DEG C, less than 100
℃。
Preferably, the shared part by weight in the nonvolatile component of inorganic agent of above-mentioned polyoxyalkylene alkyl ether be 3~
70 weight %.
Preferably, kinematic viscosity at 25 DEG C of above-mentioned polyoxyalkylene alkyl ether ester is 10mm2/ more than s, it is less than
100mm2/s。
Preferably, the shared part by weight in the nonvolatile component of inorganic agent of above-mentioned polyoxyalkylene alkyl ether ester is 1
~50 weight %.
Preferably, inorganic agent of the invention contains above-mentioned polyoxyalkylene alkyl ether and above-mentioned polyoxyalkylene alkyl ether
Ester.
Preferably, above-mentioned synthetic fibers inorganic agent is also containing selected from by alkyl sulfonic ester salt, alkyl phosphate salt, alkyl
At least one in the group of succinate salt, alkyl sulfate salt, fatty acid soaps and alkyl imidazoline salt composition.
Preferably, above-mentioned synthetic fibers are polyester fiber, Fypro or polypropylene fibre.
It is highly preferred that above-mentioned synthetic fibers inorganic agent is friction false twist using.
Synthetic fiber filament yarn line of the invention is (raw material) synthetic fiber filament yarn line is attached to synthesis of the invention
The material of fiber inorganic agent.
The manufacture method of false twist processing yarn of the invention includes the conjunction to being attached with synthetic fibers inorganic agent of the invention
Heated into fiber filament yarn, stretched, the operation of false twisting processing.
Invention effect
For containing the polyoxy Asia represented from the polyoxyalkylene alkyl ether represented by formula (1) and by following formulas (2)
At least one synthetic fibers inorganic agent of the invention selected in alkyl-alkyl ether-ether, product stability when low temperature is taken care of
It is excellent, and the stability of emulsion of inorganic agent is excellent.If the synthesis for imparting synthetic fibers inorganic agent of the invention is fine
Dimension filament yarn, then inorganic agent uniformly adheres to, therefore burr, broken yarn are few.If the manufacturer of false twist processing yarn of the invention
Method, then inorganic agent uniformly adheres to, therefore burr, broken yarn are few.
Specific embodiment
[polyoxyalkylene alkyl ether represented by formula (1)]
First, the polyoxyalkylene alkyl ether represented by following formulas (1) is illustrated.
RO-(EO)a-[(PO)b/(EO)c]-(EO)d-H (1)
(wherein, R represents the alkyl or alkenyl of carbon number 1~30, can be by any structure structure in straight or branched
Into.PO represents oxygen propylidene, and EO represents oxygen ethylidene.A, b, c and d represent each average addition molal quantity, a=1~10, b=1
~10, c=1~10, d=1~40.[(PO)b/(EO)c]) it is that b moles of PO gathers with obtained from c moles of the random additions of EO
Oxyalkylene.)
As the average addition molal quantity a in formula (1), it is not particularly limited, usually 1~10 mole, preferably 2~
6 moles, more preferably 3~4 moles.If the average addition molal quantity a in formula (1) is 1~10, hydrophily increases
Plus, therefore the emulsion intercalation method of synthetic fibers inorganic agent is excellent.
As average addition molal quantity b and c in formula (1), it is not particularly limited, b is usually 1~10 mole, preferably
It is 2~8 moles, more preferably 3~4 moles, and, c is usually 1~10 mole, preferably 2~8 moles, further excellent
Elect 3~6 moles as.In the central portion of the strand of polyoxyalkylene alkyl ether, PO and EO are randomly present, so that crystallinity drops
It is low, fusing point reduction, therefore estimate the low-temperature stability raising of synthetic fibers inorganic agent.
Average addition molal quantity d in formula (1) is not particularly limited, and usually 1~40 mole, preferably 2~30 rub
You, more preferably 3~20 moles, most preferably 4~10 moles.There is EO in the terminal part of strand, so that hydrophily
Increase, emulsifying ability is improved, therefore the emulsion intercalation method of synthetic fibers inorganic agent is excellent.
The weight average molecular weight of the polyoxyalkylene alkyl ether represented by formula (1) for 500~4000, preferably 550~
2500, particularly preferably 600~1000.In the case where weight average molecular weight is less than 500, when carrying out hot place in false twisting manufacturing procedure
During reason, smoke is produced because molecular weight is low, it is possible to the reason for being polluted as heater.In weight average molecular weight more than 4000
In the case of, molecular weight is high to cause viscosity to increase, therefore when inorganic agent is attached on synthetic fibers, coefficient of kinetic friction increase,
The reason for being likely to become burr, broken yarn.
It should be noted that weight average molecular weight refers to, the high speed gel permeation chromatography device manufactured using Tosoh (strain)
HLC-8220GPC, is injected in splitter KF-402HQ, KF-403HQ that Showa electrician (strain) is manufactured with sample solution concentration 3mg/cc,
The peak-peak measured by RI detectors.
[manufacture method of the polyoxyalkylene alkyl ether represented by formula (1)]
As the manufacture method of the polyoxyalkylene alkyl ether represented by formula (1), it is not particularly limited, can be using public affairs
The method known.For example, the manufacture method of polyoxyalkylene alkyl ether of the invention can be by：To what is represented by following formulas (A)
Alcohol only supplies oxirane, makes its operation (hereinafter referred to as first paragraph) for carrying out addition reaction；After first paragraph, epoxy is supplied
Ethane and expoxy propane, make its operation (hereinafter referred to as second segment) for carrying out random addition reaction；And it is last, only supply ring
The operation (hereinafter referred to as the 3rd section) of oxidative ethane, is carried out continuously, it is also possible to reclaim what each operation was obtained from first paragraph to the 3rd section
Accessory substance, carries out continuation reaction.
ROH (A)
As monohydric alcohol, can include：Aliphatic monohydric alcohol.Used from cost, reactivity and as synthetic fibers
From the viewpoint of the flatness of inorganic agent, the monohydric alcohol of preferred aliphat.Monohydric alcohol is preferably primary alconol or secondary alcohol, further preferably
It is primary alconol.Can be straight-chain, or side chain additionally, being alkyl as the residue after hydroxyl is removed from monohydric alcohol, can
Being saturation, or undersaturated.From the viewpoint of product stability when being taken care of from the low temperature of fiber inorganic agent,
The carbon number of monohydric alcohol preferably 4~24, more preferably 8~22, further preferred 8~18.
As above-mentioned monohydric alcohol, for example, can include：It is methyl alcohol, ethanol, propyl alcohol, butanol, amylalcohol, hexanol, enanthol, pungent
Alcohol, nonyl alcohol, decyl alcohol, tip-nip, dodecanol, tridecanol, tetradecanol, pentadecanol, hexadecanol, heptadecanol,
Octadecanol, nonadecanol, eicosanol, heneicosane alcohol, tadenan, tricosanol, tetracosanol, 25
The straight chain alcohols such as alkanol, hexacosanol, heptacosanol, n-octacosanol, nonacosanol and triacontanol；2- ethyl hexyls
Alcohol, 2- propyl enanthols, 2- butyl octanol, 1- methyl heptadecanol, 2- hexyls octanol, 1- hexyls enanthol, isodecanol, different tridecane
The branched-chain alcohos such as alcohol, 3,5,5- trimethyl hexanols；Hexenol, heptenol, matsutake alcohol, nonenol, decenol, undecylenic alcohol, 12
Enol, tridecylene alcohol, tetradecene alcohol, ten 5 enols, hexadecylene alcohol, ten 5 enols, hexadecylene alcohol, ten 5 enols, oleic alcohol,
19 enols, icosa alkene alcohol, docosene alcohol, two tetradecene alcohol, pentacosa alkene alcohol, cerotene alcohol, 27 enols, 20
The branch alkenols such as eight enols, 29 enols and 30 enols；Dissident's enol, 2- methylhexenes alcohol, different tridecylene alcohol, 1- methyl
Branch alkenols such as ten 5 enols, 1- hexyls amylalcohol, different tridecylene alcohol and different oleic alcohol etc..These alcohol can be using a kind or simultaneously
Use two or more.As the concrete example of alcohol product, it is not particularly limited, for example, can includes：Coconut alcohol, palmityl alcohol etc. come from
The higher alcohol of natural oil, KALCOL series (flower king manufacture), CONOL series (new Japan Chemical manufacture), OXOCOL series (association
Manufactured with fermentation chemistry), NEODOL series (Shell chemistry manufacture), ALFOL series (Sasol manufactures), EXXAL series (Ai Ke
Gloomy Mobil manufacture) etc..These higher alcohol products can be used alone or in combination with two or more kinds.
Wherein, preferably butanol, octanol, nonyl alcohol, decyl alcohol, dodecanol, tridecanol, tetradecanol, hexadecanol, 18
Alkanol, nonadecanol, oleic alcohol, preferably butanol, octanol, decyl alcohol, dodecanol, tridecanol, tetradecanol, hexadecane
Alcohol, octadecanol, oleic alcohol.
The manufacture method of the polyoxyalkylene alkyl ether represented by formula (1) can be carried out in the presence of a catalyst.Make
It is catalyst, is not particularly limited, for example, can includes：NaOH, potassium hydroxide, cesium hydroxide, calcium hydroxide, hydrogen-oxygen
Change the hydroxide of alkali (great soil group) metals such as barium, strontium hydroxide；Potassium oxide, sodium oxide molybdena, calcium oxide, barium monoxide, magnesia, oxidation
The oxide of the alkali such as strontium (great soil group) metal；The alkali metal such as metallic potassium, metallic sodium；The metal hydroxide such as NaOH, potassium hydroxide
Thing；The carbonate of the alkali such as sodium carbonate, sodium acid carbonate, potassium carbonate (great soil group) metal；The alkali such as sodium sulphate, magnesium sulfate (great soil group) metal
Sulfate；The organic sulfonic acids such as methanesulfonic acid, TFMS；The aromatic sulphonates such as paratoluenesulfonic acid sodium salt, p-methyl benzenesulfonic acid pyridine；
The amines such as MEA, diethanol amine, single Propanolamine, dipropanolamine, tripropanol amine, triethylamine；Iron powder, aluminium powder, antimony powder,
Aluminium chloride, aluminium bromide, iron chloride, ferric bromide, cobalt chloride, antimonous chloride, antimony chloride, antimonous bromide, butter of tin, four chlorinations
The lewis acids such as titanium, boron trifluoride, boron trifluoride Anaesthetie Ether；Sulfuric acid, the excessively Bronsted acid such as chloric acid；Potassium perchlorate, sodium perchlorate,
Cross the perchlorate of the alkali such as calcium chlorate, magnesium perchlorate (great soil group) metal；The alkali such as calcium methoxide, caustic alcohol, lithium ethoxide (great soil group) metal
Alkoxide；The phenoxide of the alkali such as potassium phenate, calcium phenoxide (great soil group) metal；Sodium metasilicate, potassium silicate, sodium aluminosilicate, aluminium silicon
The silicate such as sour potassium, sodium metasilicate, adjacent sodium metasilicate, zeolite；Aluminum hydroxide/magnesium sintered body, the magnesia of addition metal ion, burning
The Al-Mg such as hydrotalcite processed system complex oxides or these surface modifier, Lanthanide Complexes etc..These catalyst can make
With a kind or and use two or more.
The usage amount of catalyst is not particularly limited, relative to 100 weight portion alcohol, preferably 0.001~10 weight portion, more
It is preferred that 0.001~8 weight portion, further preferred 0.01~6 weight portion, particularly preferred 0.05~5 weight portion, most preferably 0.05~
3 weight portions.If the usage amount of catalyst is less than 0.001 weight portion, addition reaction sometimes can not be carried out fully, the opposing party
Face, if the usage amount of catalyst is more than 10 weight portions, it is possible to which polyoxyalkylene alkyl ether is easily coloured.
The manufacture method of the polyoxyalkylene alkyl ether for being represented by formula (1), preferably puts the raw materials such as alcohol, catalyst
Enter in reaction vessel, treatment, dewater treatment then are de-gassed to the reaction vessel.Degassing process is for example with degassing side of depressurizing
Formula, vacuum outgas mode etc. are carried out.Additionally, dewater treatment is for example with thermal dehydration mode, decompression dehydration mode, vacuum dehydration side
Formula etc. is carried out.
The manufacture method of the polyoxyalkylene alkyl ether for being represented by formula (1), does not limit especially its version
It is fixed, can be continous way, or batch-type.It is not particularly limited for reaction vessel, for example, can be included：Possess and stir
Mix groove profile reaction vessel, microreactor of blade etc..It is not particularly limited as stirring vane, can be included：Maximum leaf
Piece (MaxBlend) blade, top set (Tornado) blade, general energy (Full Zone) blade etc..
The manufacture method of the polyoxyalkylene alkyl ether for being represented by formula (1), can make addition reaction from decompression shape
State starts, it is also possible to since atmospheric pressure state, can also be since pressurized state.From atmospheric pressure state or pressurized state
In the case of beginning, preferably carried out under the atmosphere of inert gas (not active gases).If addition reaction is in inert gas
Carried out under atmosphere, then can fully remove the side reaction etc. due to the alkylene oxides such as oxirane or expoxy propane and oxygen and produce
Impurity, and consider also useful from a security point, therefore preferably.It is not particularly limited as inert gas, for example may be used
To include：Nitrogen, argon gas, carbon dioxide etc..These inert gases using a kind or and can use two or more.For
The oxygen concentration in reaction vessel under the atmosphere of inert gas is not particularly limited, preferably below 10 volume %, more preferably 5
Below volume %, more preferably below 3 volume %, particularly preferably below 1 volume %, most preferably 0.5 volume % with
Under.If oxygen concentration in reaction vessel is more than 10 volume %, there is the situation that can not fully remove impurity, and from safety
It is also not preferred from the viewpoint of property.
It is not particularly limited for the initial stage pressure in reaction vessel, for example, it is preferable to gauge pressure is 0~0.50MPa, more preferably
0~0.45MPa, further preferred 0~0.40MPa, most preferably particularly preferred 0~0.35MPa, 0~0.3MPa.If reaction is held
Initial stage pressure in device is less than 0MPa, then there is the increased situation of generating capacity of impurity.On the other hand, if in reaction vessel
More than 0.5MPa, then there is reaction speed has slack-off situation to initial stage pressure.
Pressure during addition reaction in reaction vessel is subject to oxirane, the feed speed of expoxy propane, reaction temperature, urges
The influence of agent amount etc..The pressure in reaction vessel during addition reaction is not particularly limited, and preferably gauge pressure is 0~5.0MPa,
More preferably 0~4.0MPa, more preferably 0~3.0MPa, particularly preferably 0~2.0MPa, most preferably 0.1~
1.0MPa.If pressure during addition reaction in reaction vessel is less than 0MPa, there is the slack-off situation of reaction speed.The opposing party
Face, if pressure during addition reaction in reaction vessel has the difficult situation of manufacture more than 5.0MPa.
As oxirane, the reaction temperature of the addition reaction of expoxy propane, it is not particularly limited, preferably 70~240
DEG C, more preferably 80~220 DEG C, more preferably 90~200 DEG C, particularly preferably 100~190 DEG C, most preferably 110~
180℃.If reaction temperature is less than 70 DEG C, there is the situation that can not fully carry out addition reaction.On the other hand, if reaction
Temperature is more than 240 DEG C, then poly- in the coloring and polyoxyalkylene alkyl ether of the polyoxyalkylene alkyl ether for being obtained in the presence of promotion
The situation of the decomposition of oxyalkylene.
The time (reaction time) that above-mentioned addition reaction needs is not particularly limited, preferably 0.1~100 hour, more excellent
Elect as 0.1~80 hour, more preferably 0.1~60 hour, particularly preferably 0.1~40 hour, most preferably 0.5~30
Hour.If the reaction time is less than 0.1 hour, there is the situation that addition reaction can not be carried out fully.On the other hand, if instead
More than 100 hours between seasonable, then there is the situation of production efficiency variation.
If the supply of oxirane, expoxy propane terminates, the internal pressure in reaction vessel is because of oxirane, expoxy propane
Consumption and slowly reduce.Oxirane, the addition reaction of expoxy propane proceed, until confirming that internal pressure is not changed in.Ring
Oxidative ethane, the addition reaction of expoxy propane preferably confirm the time point that internal pressure is not changed within a certain period of time, terminate reaction.Root
According to needs, it is also possible to implement heating decompression operation etc., and reclaim unreacted oxirane, expoxy propane.
In oxirane, the addition reaction of expoxy propane, atent solvent can be used as needed.For example, making as alcohol
With 30 enol (Japanese：ト リ ア U Application セ ノ ー Le) etc. under normal temperature in the case of solid matter, it is molten in advance before preferably reacting
Solution is used in atent solvent such that it is able to is fully improved reactivity, and is improved operability.Additionally, using atent solvent,
Removal effect can be expected.
It is not particularly limited as atent solvent, for example, can be included：Ether, ethylene glycol dimethyl ether, dioxs, four
The ethers such as hydrogen furans；The esters such as diethylene acetic acid esters, methyl proxitol acetate；Acetone, methylisobutylketone, first
The ketones such as base ethyl ketone；Sulfolane, dimethyl sulfone sulfoxide (Japanese：ジ メ チ Le ス Le ホ Application ホ キ シ De) etc. sulfone class；Dichloro
The halogenated hydrocarbons such as methane, chloroform；Benzene,toluene,xylene etc. is aromatic hydrocarbon；The fat such as pentane, hexane, pentamethylene, hexamethylene
Race's hydro carbons etc., it is possible to use a kind and is used two or more.Wherein, optimization aromatic hydro carbons, more preferably toluene.
As atent solvent (Japanese：Not active solvent) usage amount, be not particularly limited, used in order to dissolve alcohol
In the case of, relative to the alcohol of 100 weight portions, preferably 10~1000 weight portions, more preferably 10~500 weight portions are further excellent
Select 10~400 weight portions, most preferably particularly preferred 10~300 weight portion, 10~200 weight portions.If the amount phase of atent solvent
For 100 weight portion alcohol more than 1000 weight portions, then existing cannot fully carry out the situation of addition reaction.On the other hand, if
The amount of atent solvent is less than 10 weight portions, then existing cannot fully dissolve the situation of alcohol.It should be noted that molten using inertia
In the case of agent, removed preferably after addition reaction.By the removing of atent solvent, it is prevented from because of the residual of atent solvent
The generation of caused impurity, can obtain the polyoxyalkylene alkyl ether of various physical properties excellents.The removal step of solvent is as be described hereinafter.
After oxirane, the addition reaction of expoxy propane terminate, as needed, catalyst is preferably neutralized and/or removes,
Remove atent solvent.
The neutralization of catalyst can be carried out using usual way, such as when catalyst is base catalyst, preferably add salt
The acid of acid, phosphoric acid, acetic acid, lactic acid, citric acid, butanedioic acid, acrylic acid, methacrylic acid etc. is carried out.
The neutralization of catalyst is preferably carried out under the atmosphere of inert gas.It is not particularly limited as inert gas, for example
Can include：Nitrogen, argon gas, carbon dioxide etc., it is possible to use a kind and is used two or more.
As catalyst neutralization when temperature, be not particularly limited, preferably 50~200 DEG C, more preferably 50~190
DEG C, more preferably 60~180 DEG C, most preferably 60~160 DEG C.If the temperature during neutralization of catalyst is less than 50 DEG C,
Then in the presence of the situation that the time required for neutralization is elongated.On the other hand, if the temperature during neutralization of catalyst is more than 200 DEG C,
Then in the presence of the decomposition of the polyoxy alkylidene in the coloring and polyoxyalkylene alkyl ether of the polyoxyalkylene alkyl ether for promoting to obtain
Situation.
The pH of the reaction product obtained from above-mentioned addition reaction is adjusted to 4 preferably by the neutralization of catalyst~
10, more preferably 5~8, particularly preferably 6~8.Additionally, in catalyst and when, as needed, can be used together quinones or
The antioxidants such as phenols.
The neutralization salt generated by neutralization can again carry out separation of solid and liquid.As the solid-liquid of the neutralization salt generated after neutralization
The method of separation, can include：Filtering and centrifugation etc..Filtering for example uses filter paper, filter cloth, cartridge filter, fiber
2 layers of filter, metallic screen type filter, metal sintering type filter of element and polyester etc., under decompression or pressurization, temperature 20
Carried out under conditions of~140 DEG C.Centrifugation can for example be entered using whizzers such as precipitate and separate device or centrifugal separators
OK.Additionally, as needed, relative to the water that the weight portion of liquid 100 before separation of solid and liquid can add about 1~30 weight portion.Make
It is above-mentioned separation of solid and liquid, when particularly being filtered, the rate of filtration can be improved using filtration adjuvant, therefore be adapted to.
As filtration adjuvant, it is not particularly limited, each series of such as diatomite, hyflosuper-cell, cellpure
(Adcanced Minerals Corporation manufactures), silica #645, silica #600H, silica#600S, silica#
The diatomite such as 300S, silica#100F (central silica company manufacture), dicalite (manufacture of グ レ フコ companies)；
The perlites such as rokaheip (manufacture of mining company of Mitsui Metal Co., Ltd.), topcon (manufacture of Showa chemical company)；KC block (Japan
Paper company processed manufacture), the cellulose-based filtration adjuvant such as fibracell (Advanced Minerals Corporation manufactures)；
Silica gels such as sylopute (manufacture of SILYSIA chemical companies of Fuji) etc..These filtration adjuvants using a kind or can be used in combination
Two or more.
Filtration adjuvant can form the pre-coating method of filtration adjuvant layer using the advance filtering surface in filter paper etc., it is also possible to make
With the body feed method directly added to filtrate, it is also possible to and use both approaches.As the usage amount of filtration adjuvant, relative to
The weight portion of liquid 100 before separation of solid and liquid, more preferably preferably 0.01~5 weight portion, 0.1~1.5 weight portion.Additionally, mistake
Filter processing speed depends on size, degree of decompression or pressurization degree, treatment humidity of filter area etc., but preferably 100kg/m2·hr
More than, more preferably 300kg/m2More than hr, more preferably 500kg/m2More than hr.
Removing for catalyst is not particularly limited, for example, it is preferable to after Catalyst Adsorption is made to adsorbent, enter
The method of row separation of solid and liquid.
As adsorbent, for example, can include：The silicate of alumina silicate, magnesium silicate etc., atlapulgite, Emathlite,
Silica gel, ion exchange resin etc..As commercially available adsorbent, for example, can include：(the consonances of Kyowaad 600,700
Chemical company manufacture), Mizukalife P-1, P-1S, P-1G, F-1G (manufacture of marshy land chemical company), Tomita AD600,
The silicate such as 700 (manufactures of Fu Tian drugmakers)；Amberlyst (manufacture of Rohm＆Hass companies), Amberlite (Rohm＆
Hass companies manufacture), Diaion (Mitsubishi Chemical Ind's manufacture), Dowex (Dow Chemical's manufacture) plasma exchanger resin
Deng.These adsorbents and can also use two or more using a kind.
The usage amount of adsorbent for example relative to 100 part by weight of catalyst, preferably 100~5000 weight portions, more preferably
300~3000 weight portions.
It is not particularly limited as the removing condition of catalyst, for example, can be enumerated：In appointing for decompression, normal pressure or pressurization
Carried out under meaning pressure condition, carry out stirring mixing in 5~120 minutes to adsorbent at 20~140 DEG C of temperature, afterwards, will adsorbed
The method that the adsorbent for having catalyst by above-mentioned solid-liquid separating method separate；Adsorbent is filled in post etc. in advance,
Make reactant mixture at 20~140 DEG C of temperature by with adsorption catalyst, so that remove the method for catalyst etc..Now, root
According to needs, relative to 100 weight portion reactant mixtures, the water-soluble solvents such as lower alcohol with water or ethanol as representative can be added
1~20 weight portion.
Residual quantity after the removing of catalyst is not particularly limited, preferably below 300ppm, more preferably 200ppm with
Under, more preferably below 100ppm, particularly preferably below 50ppm, most preferably below 20ppm.
The removing of atent solvent is carried out preferably for example by distillation.
It should be noted that when the neutralization and/or removing and the removing of atent solvent of catalyst is carried out, each operation
Order is not particularly limited, if for example carrying out the neutralization of catalyst and/or the removing of atent solvent being carried out after removing,
The purification efficiency of the polyoxyalkylene alkyl ether for arriving is excellent, therefore preferably.
The manufacture method of the polyoxyalkylene alkyl ether for being represented by formula (1), the alcohol remained as unreacted contains
Amount, is not particularly limited, more excellent below preferably 1 weight portion relative to the weight portion of polyoxyalkylene alkyl ether 100 for obtaining
Elect as below 0.01 weight portion, below more preferably 0.001 weight portion, below particularly preferably 0.0001 weight portion, most
Below preferably 0.00001 weight portion.If unreacted and the alcohol content that remains are relative to 100 weight portion polyoxyalkylene alkyls
Then there is smelly situation more than 1 weight portion in ether.
[cloud point of the 1 weight % aqueous solution of the polyoxyalkylene alkyl ether represented by formula (1)]
The cloud point of the 1 weight % aqueous solution of the polyoxyalkylene alkyl ether represented by formula (1) is preferably more than 60 DEG C, more
Preferably more than 70 DEG C, more preferably more than 75 DEG C, according to this sequentially, the stability of emulsion of inorganic agent is improved.Preferably
Higher limit is less than 100 DEG C.If less than 60 DEG C, then the emulsion stability with inorganic agent is deteriorated.
[fusing point of the polyoxyalkylene alkyl ether represented by formula (1)]
The fusing point of the polyoxyalkylene alkyl ether represented by formula (1) is preferably less than 15 DEG C, more preferably less than 10 DEG C,
More preferably less than 8 DEG C, most preferably less than 5 DEG C, according to this sequentially, the low-temperature stability of fiber inorganic agent is improved.
Preferred lower limit is -30 DEG C, and more preferably lower limit is -20 DEG C, and further preferred lower limit is -10 DEG C.If it exceeds 15 DEG C,
According to storage condition (for example, winter of low temperature), there is the situation that the composition of inorganic agent is separate.
[the polyoxyalkylene alkyl ether ester represented by formula (2)]
Then, the polyoxyalkylene alkyl ether ester represented by following formulas (2) is illustrated.
R1O-(EO)e-[(PO)f/(EO)g]-(EO)h-CO-R2 (2)
(wherein, in formula (2), R1The alkyl or alkenyl of carbon number 1~30 is represented, can appointing by straight chain or side chain
One structure is constituted.R2The alkyl or alkenyl of carbon number 1~30 is represented, can be made up of any structure of straight or branched.PO
It is oxygen propylidene, EO is oxygen ethylidene.E, f, g and h represent each average addition molal quantity, e=1~10, f=1~10, g=1
~10, h=1~40.[(PO)f/(EO)g] it is f moles of PO and polyoxy alkylidene obtained from g moles of the random additions of EO.)
The polyoxyalkylene alkyl ether ester represented by formula (2) is that have with aliphatic acid to described above by formula (1)
The polyoxyalkylene alkyl ether of expression be esterified after structure compound.Therefore, the R of formula (2)1, e, f, g, h and formula
(1) R, a, b, c, d is corresponded to respectively.That is, R1Corresponding to R, e corresponds to a, and f corresponds to b, and g corresponds to c, and h corresponds to d.Formula
(2) R1, e, f, g, h preferred scope it is identical with R, a, b, c, d of formula (1).
R2It is from aliphatic acid (R2COOH) except the residue after decarboxylate.R2Carbon number be preferably 3~23, more preferably 5
~19, more preferably 7~17.R2It is preferred that primary alkyl or alkenyl.
As the aliphatic acid (R for being esterified to the polyoxyalkylene alkyl ether represented by formula (1)2COOH), example
Can such as include：It is acetic acid, propionic acid, butyric acid, caproic acid, octanoic acid, capric acid, laurate, myristic acid, palmitic acid, palmitoleic acid, hard
Resin acid, isostearic acid, oleic acid, linoleic acid, leukotrienes, behenic acid, erucic acid, tetracosanoic acid etc..These aliphatic acid can use a kind
And two or more can also be used.As the specific example of fatty acid product, it is not particularly limited, for example, can includes：LUNAC
Series (flower king manufacture).Wherein, from from the viewpoint of lubricity, more preferably octanoic acid, capric acid, laurate, myristic acid, palm
Acid, stearic acid, isostearic acid, oleic acid.
As the manufacture method of the polyoxyalkylene alkyl ether ester represented by formula (2), it is not particularly limited, can uses
Known method.For example, as described above, after the polyoxyalkylene alkyl ether that manufacture is represented by formula (1), according to public affairs
The method known, using aliphatic acid (R2COOH) it is esterified such that it is able to the polyoxyalkylene alkyl that manufacture is represented by formula (2)
Ether-ether.
[kinematic viscosity of the polyoxyalkylene alkyl ether ester represented by formula (2)]
The kinematic viscosity of the polyoxyalkylene alkyl ether ester represented by formula (2) is preferably 10~100mm2/ s, more preferably
It is 10~80mm2/ s, further preferred 10~50mm2/ s, most preferably 20~40mm2/s。
If less than 10mm2/ s, then the viscosity of inorganic agent is too low, and flying for inorganic agent is likely to occur in oil supply operation
Dissipate.If additionally, in 100mm2/ more than s, then the viscosity of inorganic agent uprise, to synthetic fiber filament yarn line autgmentability be deteriorated,
Therefore, to the tack possible deviation of fiber.
[synthetic fibers inorganic agent]
Synthetic fibers inorganic agent of the invention must contain from the polyoxyalkylene alkyl ether represented by formula (1) and by
At least one selected in the polyoxyalkylene alkyl ether ester that following formulas (2) represent.By the way that such composition must be contained, from
And effect of the invention can be played.
Must be containing in the case of above-mentioned polyoxyalkylene alkyl ether, polyoxyalkylene alkyl ether is in the non-volatile of inorganic agent
Shared part by weight is preferably 3~70 weight %, more preferably 5~65 weight %, more preferably 10~60 weights in composition
Amount %, most preferably 15~55 weight %.If less than 3 weight %, then the cloud point of the emulsion of inorganic agent is low, it is possible to separate, such as
Fruit is possible to be deteriorated more than 70 weight %, then flatness or convergence.
It should be noted that nonvolatile component of the invention refers to, inorganic agent is heat-treated at 105 DEG C, removed
The volatile ingredients such as solvent, reach over dry composition during constant.
In the case of must be containing above-mentioned polyoxyalkylene alkyl ether ester, polyoxyalkylene alkyl ether ester be in inorganic agent
Shared part by weight is preferably 1~50 weight %, more preferably 1~40 weight %, more preferably 3 in nonvolatile component
~30 weight %, most preferably 5~20 weight %.If less than 3 weight %, then the tack of inorganic agent, lubricity may become
Difference, if it exceeds 50 weight %, then the cloud point of the emulsion of inorganic agent is low, and inorganic agent may possibly be separated.
Additionally, inorganic agent of the invention is preferably comprised by the polyoxyalkylene alkyl ether of formula (1) expression and by formula (2)
The polyoxyalkylene alkyl ether ester of expression.The two compositions must be contained, so that the viscosity reduction of inorganic agent, can be by inorganic agent
It is evenly affixed to fiber.As a result, burr, the broken yarn produced in yarn operation processed and manufacturing procedure can be reduced further.
And weight ratio (the polyoxy Asia of polyoxyalkylene alkyl ether during with the two compositions and polyoxyalkylene alkyl ether ester
Alkyl-alkyl ether：Polyoxyalkylene alkyl ether ester) it is preferably 20:80~99:1, more preferably 40:60~95:5, it is further excellent
Elect 55 as:45~90:10.
In the case where synthetic fibers inorganic agent of the invention contains polyoxyalkylene alkyl ether and polyethers, inorganic agent
Product stability when low temperature is taken care of improves effect and the stability of emulsion raising effect of inorganic agent is easier to play.For this hair
Bright synthetic fibers inorganic agent, polyoxyalkylene alkyl ether and the shared weight ratio in the nonvolatile component of inorganic agent of polyethers
Example is preferably more than 30 weight %, more preferably more preferably more than 35 weight %, most preferably more than 40 weight %, 50 weights
Amount more than %.According to this sequentially, the product stability when low temperature of inorganic agent is taken care of improves the emulsion-stabilizing of effect and inorganic agent
Property improve effect be readily obtained.Polyoxyalkylene alkyl ether and polyethers synthetic fibers inorganic agent of the invention it is non-volatile into
The higher limit of shared part by weight is preferably below 100 weight % in point, more preferably below 95 weight %, further preferably
It is below 90 weight %.
Synthetic fibers inorganic agent of the invention considers from following viewpoints, is particularly suitable as the friction false twist of synthetic fibers
Use inorganic agent.
Generally, false twist processing yarn (Draw Texturing Yarn：Hereinafter, it is abbreviated as DTY), it is to assign friction false twist to use
Inorganic agent and production section orientated yarns (Partially Oriented Yarn：Hereinafter abbreviated as POY) after, then by adding
Thermal (heater) is heated to yarn, stretch so as to obtain while yarn is twisted by false-twisting device
Arrive.
Now, the imparting amount of friction false twist inorganic agent is more, burr, broken yarn, the white of the operation generation of false twisting processing
Powder, the problem of stain can more be inhibited, but friction false twist inorganic agent on heater (heater) is de-
The amount that falls increases.Therefore, friction false twist inorganic agent can pollute heater, and heater is cleaned needs plenty of time and work
Power, can cause productivity to reduce.
Therefore, the imparting amount of synthetic fibers inorganic agent is commonly angled relative to (raw material) synthetic fibers for 1.0 weight %, with this
Relatively, the imparting amount of friction false twist inorganic agent is designed to low to 0.25~0.80 weight %.Understand from the above fact, friction
False twisting inorganic agent is low to the imparting amount on the synthetic fibers, therefore more important to the uniform tack of fiber.
In recent years, as using which processing yarn species, have surcharge fine denier yarn high, full-dull yarn,
The increased tendency of production of special yarn as gloss odd-shaped cross section yarn.Generally, be susceptible to known to these special yarns fiber with
The boundling of fiber that the friction produced between roller, fiber and guide, fiber and false twist unit, fiber causes is bad, tension force change
Dynamic, antistatic bad etc. problem.Such special yarn kind easily produces Soft flocks, therefore cannot productivity is good obtains
The false twist processing yarn of high-quality.
That is, for produce in recent years it is increased easily cause the kind of burr, broken yarn, white powder, stain, abundant
Suppress burr, broken yarn, white powder, stain and prevent from putting aside the aspect of pollution on the heaters, be not satisfied with also
Result.
Synthetic fibers inorganic agent of the invention as the friction false twist used time, by stability and the place of improving inorganic agent
The emulsion intercalation method of agent is managed, so that the uniform tack to fiber is significantly improved, in the false twist processing yarn of synthetic fibers
Production in, can reduce false twisting processing operation in produce burr, broken yarn, white powder, stain imperfect manufacture,
And the cleaning period of heater can be extended.
Additionally, synthetic fibers inorganic agent of the invention is not being damaged in the range of effect of the invention, as needed,
Lubricant, emulsifying agent, penetrant, antistatic additive etc. can be contained.Improved from the convergence for further embodying fiber and oil film is strong
From the viewpoint of the characteristic of change, the nonvolatile component for being aggregated in inorganic agent of lubricant, emulsifying agent, bleeding agent, antistatic additive etc.
In shared part by weight be preferably below 50 weight %, more preferably below 40 weight %, more preferably 30 weight %
Hereinafter, most preferably below 20 weight %.
As lubricant, it is not particularly limited, it is possible to use known lubricant.Can for example enumerate：Methyl oleate, palm fibre
The different monooctyl ester of palmitic acid acid butyl ester, butyl stearate, butyl oleate, laurate, isobutyl palmitate, Ethylhexyl stearate, oleic acid are different pungent
Ester, laurel oleate, stearic acid isotridecyl ester, cetyl stearate, oleic acid isostearate, sad grease, the moon
The fatty acid ester compounds such as cinnamic acid grease, palmitic acid grease, stearic acid lipid, oleic acid grease (monohydric alcohol with it is monocarboxylic
Ester)；Diethylene glycol dilaurate, diethylene glycol dioleate, hexylene glycol dilaurate, hexylene glycol dioleate, new penta
Glycol dilaurate, trimethylolpropane tris caprylate, trimethylolpropane trilaurate, trimethylolpropane tris palm
Acid esters, trimethylolpropane tris oleate, glycerol trioleate, the laurate of pentaerythrite four, the oleate of pentaerythrite four etc.
Polyalcohol and monocarboxylic ester；The oil base ester of maleic acid two, the isotridecyl ester of adipic acid two, the cetyl of adipic acid two, oneself two
Sour two greases, decanedioic acid dioctyl ester, decanedioic acid dilauryl, decanedioic acid distearyl base ester, azelaic acid dibutyl ester, azelaic acid two
The ester of the polybasic carboxylic acids such as stearyl ester, o-phthalic acid dibutyl ester, trioctyl trimellitate (TOTM) and monohydric alcohol；To Neodol 23
The synthol of manufacture (Shell) addition product of 2 moles of oxirane and lauric ester, 2 to the additions of NEODOL 23
The product of moles of ethylene oxide and the diester of adipic acid, the product of 2 mol propylenoxies and bay to different tridecanol addition
The ester of acid, two ends of the block of oxirane and expoxy propane or random copolymer or an end are by poly- after carboxylic acid-terminated
Alcohol after the additions such as compound alkylene oxide and ester of carboxylic acid etc..
Suitably two or more is used in combination these lubricants as needed.Lubricant is shared in the nonvolatile component of inorganic agent
Part by weight is not particularly limited, preferably 0~30 weight %, more preferably 0~10 weight %.
In order that inorganic agent emulsification, in order to aid in the tack of fiber or in order to from the fibre for being attached with inorganic agent
Dimension washing process agent, it is possible to use emulsifying agent, penetrant.As emulsifying agent, penetrant, it is not particularly limited, can be using public affairs
The material known.Can for example enumerate：Polyoxyethylenelauryl ether, polyoxy Asia second of the weight average molecular weight more than 300, less than 1000
Base oleyl ether, polyoxyethylene nonylplenyl ether etc..And also can include：Polyoxyethylenelauryl base amino ethers, poly- second
Glycol monolaurate, polyethylene glycol dilaurate, polyethylene glycol monooleate, glycol dioleate, glycerine list oil
Acid esters, sorbitan monooleate, polyoxyethylene glyceryl monolaurate, the oleic acid of polyoxy ethylene sorbitol alcohol acid anhydride three
Nonionic surfactants such as ester, polyoxyethylene castor oil ether, polyoxyethylene rilanit special ether etc., can also enumerate
Go out：Nonionic surfactants of nitrogenous system such as oleic acid diethyl amide, polyoxyethylenelauryl acid single ethanol amide etc..These
Emulsifying agent, penetrant may be used singly or two or more kinds thereof as needed.Emulsifying agent, penetrant are not waved inorganic agent
Shared part by weight is not particularly limited in hair composition, preferably 0.1~40 weight %, more preferably 0.1~30 weight
Amount %.It should be noted that these emulsifying agents, penetrant can also be in order to assign fiber yarn antistatic behaviour, assign lubricity
Used with convergence.
It is not particularly limited as antistatic additive, can be using known antistatic additive.Can for example enumerate：Alkyl phosphoric acid
The slaine/or amine salt of ester (below, being abbreviated as phosphate), the slaine/of polyoxyethylene phosphate or amine salt, alkane
The anion surfactants such as sulfonate, fatty acid soaps；The cationic surfaces such as alkylamine salt, alkyl imidazoline salt, quaternary ammonium salt
Activating agent；Amphoteric surfactantes such as Empigen, stearyl dimethyl betaine etc..These antistatic additive roots
According to needing to can be used alone or suitable and use two or more.The shared weight in the nonvolatile component of inorganic agent of antistatic additive
Amount ratio is not particularly limited, preferably 0.1~10 weight %, more preferably 0.1~5 weight %.
Beyond the compositions such as above-described lubricant, emulsifying agent, penetrant, antistatic additive, as needed, certainly can be with
Use the compositions such as antioxidant, preservative, antirust agent, defoamer.
Generally from from the viewpoint of conveying cost, the stability of inorganic agent, synthetic fibers inorganic agent of the invention is made
Imparting synthesis is transplanted on for the inorganic agent that the shared part by weight in inorganic agent of nonvolatile component is more than 80 weight % fine
Tie up the factory of long filament.For inorganic agent of the invention, the stability of inorganic agent is very good, is prevented from outward appearance not good or composition
Separate.As a result, inorganic agent can be evenly affixed to synthetic fibers, can greatly improve and be produced in yarn operation processed, manufacturing procedure
Raw problem.
Synthetic fibers of the invention inorganic agent preferably also contains outward appearance regulator.Outward appearance regulator can improve inorganic agent
Stability.Outward appearance regulator is the composition that can be volatilized by heat treatment in the manufacturing process of synthetic fibers, removed.Outward
See the shared part by weight in inorganic agent entirety of regulator and be preferably 0.1~20 weight %, more preferably 0.1~10 weight
Amount %.If the part by weight of outward appearance regulator is more than 20 weight %, as the penalty of fiber inorganic agent, in synthesis
In the production of the false twist processing yarn of fiber, it is impossible to enough reduce burr, broken yarn, white powder, the dye produced in false twisting manufacturing procedure
The manufacturing deficiency of color spot, it is possible to imperfect manufacture can be increased on the contrary.
It is not particularly limited as outward appearance regulator, can be using known outward appearance regulator.Can as outward appearance regulator
To include：Water or lower alcohol.For example, can include：Water, ethylene glycol, propane diols, isopropanol, glycerine, butanediol etc..
In these, preferably water, ethylene glycol, glycerine.Outward appearance regulator can be used alone or appropriate and use two or more as needed.
Synthetic fibers inorganic agent of the invention can be made up of the mentioned component for only including nonvolatile component, it is also possible to by
Nonvolatile component and outward appearance regulator are constituted, or dilute the material after nonvolatile component with low viscosity mineral oil, also may be used
Being the water serial emulsion after being emulsified to nonvolatile component in water.After being emulsified to nonvolatile component in water
Water serial emulsion in the case of, the concentration of nonvolatile component is preferably 5~20 weight %, more preferably 6~15 weight %, enters one
Step is preferably 8~12 weight %.
Manufacture method for synthetic fibers inorganic agent of the invention is not particularly limited, can be using known side
Method.Inorganic agent usually can mix the above-mentioned each composition for being constituted so as to manufacture with random order.
[synthetic fiber filament yarn line]
Synthetic fiber filament yarn line of the invention is to be attached to conjunction of the invention on (raw material) synthetic fiber filament yarn line
Material into after fiber inorganic agent, in the production of the false twist processing yarn of synthetic fibers, can be reduced in false twisting manufacturing procedure
The burr of middle generation, broken yarn, white powder, the manufacturing deficiency of stain, can extend the cleaning period of heater.Synthetic fibers
0.1~1.0 weight % is preferably relative to (raw material) filament of synthetic fibre with the adhesion amount of the nonvolatile component of inorganic agent, it is more excellent
Elect 0.2~0.8 weight %, more preferably 0.3~0.6 weight % as.
As the method to (raw material) filament of synthetic fibre imparting synthetic fibers inorganic agent of the invention, do not limit especially
It is fixed, can be using known method.Generally, can include：Assigned in the spinning process or stretching process of filament of synthetic fibre
Give, to (raw material) filament of synthetic fibre oiling roller, oil guiding etc. will only comprising will not send out composition inorganic agent, use low viscosity mineral
Oil nonvolatile component is diluted after inorganic agent or the water serial emulsion treatment after being emulsified to nonvolatile component in water
Agent carries out method of oil supply etc..
Synthetic fibers inorganic agent of the invention, is particularly suitable for the synthesis such as polyester fiber, Fypro, polypropylene fibre
The false twisting processing purposes of fiber.As polyester fiber, can include：It is the poly- of main Component units with para Toluic Acid's second diester
Ester (PET), with polyester (PTT) that para Toluic Acid's propylene diester is main Component units, with para Toluic Acid's fourth diester as main composition
The polyester (PBT) of unit, with polyester (PLA) that lactic acid is main Component units etc..As Fypro, can include：
Nylon 6, nylon66 fiber etc., can include as polypropylene fibre：Polypropylene etc..
[manufacture method of false twist processing yarn]
The manufacture method of false twist processing yarn of the invention includes：Synthetic fibers inorganic agent to being attached with the invention described above
Synthetic fiber filament yarn line heated, stretched, the operation of false twisting processing, the hair produced in false twisting manufacturing procedure can be reduced
Thorn, broken yarn, white powder, the manufacturing deficiency of stain, can extend the cleaning period of heater.As the side that false twisting is processed
Method, is not particularly limited, can be using known method.For example, can include：Described in WO2009/034692 publications
Method etc..
As false twisting processing conditions, it is not particularly limited, from from the viewpoint of further playing effect, preferably using makes conjunction
Directly contacted with the hot plate of thermal source into fiber filament yarn with the vacation of the contact type (hot plate contact heating means) for being heated
Twisting with the fingers processing machine carries out false twisting processing.For the false twist processing machine that such hot plate contacts mode of heating, heter temperature is 160 DEG C
~230 DEG C, heater length is 150cm~250cm, and synthetic fiber filament yarn line is contacted so as to divide a word with a hyphen at the end of a line with the surface of heating plate
Material.Firing rate is usually 500~1000m/min, preferably 600~800m/min.
【Embodiment】
Hereinafter, the present invention is illustrated by embodiment, but is not limited by the embodiment recorded herein.Need explanation
, the percentage (%) of expression is such as not particularly limited in text neutralization table, then it represents that " weight % ".Embodiment and comparative example
In, each evaluation is carried out based on method as shown below.
First, obtain as follows Production Example 1~12 and manufacture comparative example 1~12 polyoxyalkylene alkyl ether POA-1~
12 and POA-D1~12.
<Production Example 1>
To can be stirred, temperature adjustment, with alkylene oxide stuffing box, nitrogen supply pipe, the 2L of pressure adjustment pump height
In pressure kettle (autoclave), Cs of the 193g as alcohol is put into12~13Alcohol, the 0.9g potassium hydroxide as base catalyst.To autoclave
Inside carry out after nitrogen displacement, stir while carrying out 1 hour dehydrating operations at 100~110 DEG C.Then, in order to reach the phase
The molar ratio of prestige, in 0.0~0.4MPa of gauge pressure, reaction temperature at 140~150 DEG C, input 132g oxirane is used as the
, the mixture of 116g expoxy propane and 132g oxirane is put into as second segment, input 264g oxirane is used as three by one section
Section, carries out the polyaddition reaction of about 8 hours.Thereafter, in being carried out to the polyoxyalkylene alkyl ether for obtaining with 1.4g lactic acid
With process and reclaim.So, polyoxyalkylene alkyl ether (POA-1) is obtained.
<Production Example 2~12 and manufacture comparative example 1~12>
In addition to the addition molal quantity of the alcohol, oxirane and expoxy propane of each example of the record of list of modification 1~4, with system
Make example 1 same, obtain POA-2~12 and POA-D1~12.The 1 weight % aqueous solution of polyoxyalkylene alkyl ether is determined as follows
Cloud point and polyoxyalkylene alkyl ether fusing point.
<The cloud point of the 1 weight % aqueous solution of polyoxyalkylene alkyl ether>
Prepare the 1 weight % aqueous solution of polyoxyalkylene alkyl ether.Then, heating makes cloud test liquid temporarily muddy, will
The temperature that muddiness disappears is used as cloud point.
<The fusing point of polyoxyalkylene alkyl ether>
Polyoxyalkylene alkyl ether is taken with the capillary of the two ends open pipe of given size, it is close to the mercury of thermometer
Ball, is slowly heated up in air bath, and sample is melted, and temperature when being up to opaque is used as fusing point.
Table 1
Table 2
Table 3
Table 4
Then, the polyoxyalkylene alkyl ether ester of Production Example 13~18 and manufacture comparative example 13~18 is obtained as follows
POAEE-13~18 and POAEE-D13~18.
<Production Example 13>
In addition to the addition molal quantity of the alcohol, oxirane and the expoxy propane that are changed to described in table 5, with Production Example 1
Equally, polyoxyalkylene alkyl ether is obtained.Polyoxyalkylene alkyl ether to obtaining carries out esterification with aliphatic acid as follows.
In with stirring vane, heater, the reaction vessel of dehydrating tube add 775g polyoxyalkylene alkyl ethers and
248g laurate, carries out 8 hours esterifications at 180~210 DEG C.In this way, obtaining polyoxyalkylene alkyl ether ester (POAEE-
13)。
<Production Example 14~20 and manufacture comparative example 13~20>
Except the addition molal quantity and fat of the alcohol, oxirane and expoxy propane of each example described in list of modification 5~6
It is same with Production Example 13 outside acid, obtain POAEE-14~20 and POAEE-D13~20.Polyoxy alkylidene alkane is determined as follows
The kinematic viscosity of base ether-ether.
<The kinematic viscosity of polyoxyalkylene alkyl ether ester>
About 10g samples are put into Cannon-Fenske viscometer, 15 points are kept in the thermostat that temperature adjustment is 25 DEG C
Clock.Thereafter, the delivery time (second) between the graticule that sample passes through viscosimeter is determined, viscosimeter coefficient is multiplied by, the value that will be obtained is made
It is kinematic viscosity.
Table 5
Table 6
<Embodiment 1>
Then, the gradation composition that table 7 is recorded is mixed, prepares the synthetic fibers inorganic agent of embodiment 1.By its result
It is shown in table 7.
Then, to water is added in the synthetic fibers inorganic agent for preparing, the part by weight for preparing nonvolatile component is 10 weights
Measure the water serial emulsion of %.Then, be to the titanium oxide content for mouthful being sprayed and being cooled and solidified from metal with extruder 2.5% it is poly- right
Polyethylene terephthalate full-dull yarn, by using the oily guide mode of dosing pump assembly, assigns water serial emulsion, so that place
The adhesion amount for managing the nonvolatile component of agent reaches 0.6 weight %, weaving 89dtex/72f (89 デ シ テ ッ Network ス/72 Off ィ ラ メ
Application ト) POY yarns, and batched with the speed of 2800m/min, so as to obtain 10kg doff volume (Volume き チ ー ズ).Then,
Using the POY for obtaining, the false twist processing machine of mode of heating is contacted by hot plate, with following false twisting processing conditions, 10 continuous
Operating carries out draw false twisting processing, obtains false twist processing yarn (DTY).Carry out processing false twisting broken yarn, contact by following methods
Heater pollution, white powder generating capacity, the evaluation of dyeing knitted fabric spot.The results are shown in table 7.
<False twisting processing conditions>
As the draw false twisting condition of the false twist processing machine of hot plate contact mode of heating
False twist processing machine：Teijin machimery (Co., Ltd.) HTS-15V processed
Process velocity：600m/min
Draw ratio (DR)：1.60
Twist with the fingers hang device：Three reel friction mode 1-5-1
(guiding plate 1-5-guiding plate of work (polyurethane) disk 1)
Disk speed/yarn speed (D/Y)：1.8
Overrate：3%
Primary heater (twisting side) temperature：200℃
Secondary heater (backtwisting side) temperature：Room temperature
Processing number of days：10 days
<Product stability>
The synthetic fibers inorganic agent described in the embodiment and comparative example of polyoxyalkylene alkyl ether will have been coordinated 10
DEG C, 5 DEG C, place 1 week under -5 DEG C of atmosphere, the outward appearance of range estimation determination processing agent.
◎：- 5 DEG C, still homogeneous transparent after placing 1 week
○：5 DEG C, still homogeneous transparent after placing 1 week
△：5 DEG C, separated after placing 1 week
×：10 DEG C, separated after placing 1 week
<40 DEG C of stability of emulsion>
The synthetic fibers prepared in embodiment and comparative example with the stability of emulsion of inorganic agent by the transmitance of emulsion come
Evaluated.Transmitance is to place 10% concentration emulsion of synthetic fibers inorganic agent 1 week under 40 DEG C of atmosphere, is used
(strain) Hitachi spectrophotometer U-1900Spectrophotometer is measured.Condition determination is defined as wavelength
750nm, temperature of the measurement are 25 DEG C.
Transmitance is qualified more than 95%
Transmitance 100%：40 DEG C place 1 week after still homogeneous transparent
Transmitance more than 95~be less than 100%：Slightly Bluish white is transparent after being placed at 40 DEG C 1 week
Transmitance is below 95%：40 DEG C place 1 week after be gonorrhoea state
<Broken yarn is processed in false twisting>
Carry out after draw false twisting processing, broken yarn number of times is evaluated as follows.Broken yarn number of times is more, is more susceptible to burr.
◎：0 time
○：1~2 time
△：3~4 times
×：More than 5 times
<Contact heater pollutes>
Carry out after draw false twisting processing, estimate the pollution situation of heater, evaluate as follows.
◎：Heater does not pollute
○：Heater only part is contaminated
△：Heater almost half be contaminated
×：Heater is all contaminated
<White powder (Japanese：White powder) generating capacity>
Carry out after draw false twisting processing, by estimating the white powder generating capacity on navel, its periphery, be carried out as follows and comment
Valency.
◎：There is no white powder after processing on the 10th
○：Some white powder after processing on the 10th
△：Produced after processing on the 5th and pile up white powder
×：White powder is produced and piled up since processing
<Dyeing knitted fabric spot>
Carry out after draw false twisting processing, use (strain) little Chi machinery productions made round volume machine processing yarn system for obtaining
Make cylinder needle knitting, carry out the dyeing treatment of polyester knitted.The dyeability of the knitted fabric to obtaining is evaluated as follows.
◎：There is no stain
△：Confirmation has a small amount of stain
×：Confirm many stains
(embodiment 2~12, comparative example 1~12)
In addition to being changed to the gradation composition of table 7 and each example described in table 8, preparing synthetic fibers inorganic agent, with
Embodiment 1 is same, is evaluated.The results are shown in table 7 and table 8.It should be noted that polyethers 1 and polyethers in table 7~12
2 is following polyethers.
Polyethers 1：PO/EO=50/50, weight average molecular weight 5000
Polyethers 2：PO/EO=50/50, weight average molecular weight 2000
Table 7
Table 8
Knowable to table 7 and table 8, in embodiment 1~12, as long as of the invention contain the polyoxy represented by formula (1)
The synthetic fibers inorganic agent of alkylidene alkyl ether, then product stability and emulsion transmitance are excellent, false twisting processing broken yarn, contact
Seldom, yarn processed is excellent for heater pollution, white powder yield and dyeing knitted fabric spot.
On the other hand, in comparative example 1~12, due to without the polyoxyalkylene alkyl ether represented by formula (1), therefore
The effect that embodiment is obtained cannot be obtained.
(embodiment 13~18, comparative example 13~18)
Gradation composition except each example for being changed to described in table 9, prepare synthetic fibers inorganic agent in addition to, with embodiment
1 is equally evaluated.The results are shown in table 9.
Table 9
As known from Table 9, in embodiment 13~18, if of the invention contain the poly (oxyalkylene) represented by formula (2)
The synthetic fibers inorganic agent of base alkyl ether acetate, then product stability and emulsion transmitance are excellent, and false twisting processing broken yarn, contact add
Hot device pollution, white powder yield and dyeing knitted fabric spot are few, and yarn processed is excellent.
On the other hand, in comparative example 13~18, due to without the polyoxyalkylene alkyl ether ester represented by formula (2),
Therefore the effect that embodiment is obtained cannot be obtained.
(embodiment 19~30, comparative example 19~30)
In addition to being changed to the gradation composition of table 10 and each example described in table 11, preparing synthetic fibers inorganic agent,
Evaluated similarly to Example 1.The results are shown in table 10 and table 11.
Table 10
Table 11
Knowable to table 10 and table 11, in embodiment 19~30, as long as containing of the invention by gathering that formula (1) is represented
The synthetic fibers inorganic agent of oxyalkylene alkyl ether and the polyoxyalkylene alkyl ether ester represented by formula (2) of the invention,
Then product stability and emulsion transmitance are excellent, false twisting processing broken yarn, contact heater pollution, white powder generating capacity and knitting
Thing stain is few, and yarn processed is excellent.Particularly, inorganic agent can be evenly attached to fiber in these embodiments, thus it is false
Sth. made by twisting processing broken yarn is few, and burr is also few.
On the other hand, in comparative example 19~30, due to without from it is of the invention by formula (1) represent polyoxy alkylidene
Alkyl ether and at least one by being selected in the polyoxyalkylene alkyl ether ester of formula (2) expression of the invention, therefore cannot obtain
To the effect that embodiment is obtained.
Practicality in industry
The product stability when low temperature of synthetic fibers inorganic agent of the invention is taken care of is excellent, and inorganic agent emulsion
Excellent in stability, thus synthetic fibers when being produced with long filament burr, broken yarn it is few, can improve production efficiency.
Claims (9)
1. a kind of synthetic fibers inorganic agent, containing the polyoxyalkylene alkyl ether represented by following formulas (1),
RO-(EO)a-[(PO)b/(EO)c]-(EO)d-H (1)
Wherein, in formula (1), R represents the alkyl or alkenyl of carbon number 1~30, can be by any structure structure of straight or branched
Into；PO is oxygen propylidene, and EO is oxygen ethylidene；A, b, c and d represent each average addition molal quantity, a=1~10, b=1~
10, c=1~10, d=1~40；[(PO)b/(EO)c]) it is b moles of PO and polyoxy obtained from c moles of the random additions of EO
Alkylidene.
2. synthetic fibers inorganic agent according to claim 1, it is characterised in that the polyoxyalkylene alkyl ether it is molten
Point is less than 15 DEG C.
3. synthetic fibers inorganic agent according to claim 1 and 2, it is characterised in that the polyoxyalkylene alkyl ether
The 1 weight % aqueous solution cloud point for more than 60 DEG C, less than 100 DEG C.
4. synthetic fibers inorganic agent according to claim 1 and 2, it is characterised in that the polyoxyalkylene alkyl ether
Shared part by weight is 3~70 weight % in the nonvolatile component of inorganic agent.
5. synthetic fibers inorganic agent according to claim 1 and 2, it is characterised in that the synthetic fibers inorganic agent
Also contain from alkyl sulfonic ester salt, alkyl phosphate salt, alkyl acid esters salt, alkyl sulfate salt, fatty acid soaps and alkyl
At least one selected in imidazoline salt group.
6. synthetic fibers inorganic agent according to claim 1 and 2, it is characterised in that the synthetic fibers are fine polyester
Dimension, Fypro or polypropylene fibre.
7. synthetic fibers inorganic agent according to claim 1 and 2, it is characterised in that the synthetic fibers inorganic agent
It is that friction false twist is used.
8. a kind of synthetic fiber filament yarn line, it is characterised in that make synthetic fiber filament yarn line be attached in claim 1~7
Synthetic fibers inorganic agent described in any one.
9. a kind of manufacture method of false twist processing yarn, it is characterised in that including to the synthetic fiber filament yarn described in claim 8
Line is heated, stretched, the operation of false twisting processing.
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| JP2013-150479 | 2013-07-19 | ||
| JP2013150479 | 2013-07-19 | ||
| PCT/JP2014/066756 WO2015008591A1 (en) | 2013-07-19 | 2014-06-25 | Synthetic fiber treatment agent and use of same |
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| JP5881267B1 (en) * | 2015-06-25 | 2016-03-09 | 竹本油脂株式会社 | Synthetic fiber treatment liquid and synthetic fiber treatment method |
| JP6625449B2 (en) * | 2016-03-07 | 2019-12-25 | 松本油脂製薬株式会社 | Synthetic fiber treatment agent and its use |
| JP5878261B1 (en) * | 2015-06-30 | 2016-03-08 | 松本油脂製薬株式会社 | Treatment agent for synthetic fiber and its use |
| CN106319970B (en) * | 2015-06-30 | 2020-06-19 | 松本油脂制药株式会社 | Treating agent for synthetic fiber and use thereof |
| WO2017150229A1 (en) * | 2016-03-04 | 2017-09-08 | 松本油脂製薬株式会社 | Synthetic fiber treatment agent and use thereof |
| KR102355502B1 (en) * | 2018-04-16 | 2022-02-08 | 다케모토 유시 가부시키 가이샤 | Treatment agent for synthetic fibers and synthetic fibers |
| JP6386206B1 (en) * | 2018-06-15 | 2018-09-05 | 竹本油脂株式会社 | Polyolefin-based nonwoven fabric treating agent, polyolefin-based synthetic fiber, and method for treating polyolefin-based synthetic fiber |
| JP7400394B2 (en) * | 2019-11-25 | 2023-12-19 | セイコーエプソン株式会社 | Defibration method and fibrous body forming method |
| RU2746324C1 (en) * | 2020-03-26 | 2021-04-12 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ивановский государственный химико-технологический университет" | Composition for processing yarn from polyester fibers |
| JP6795238B1 (en) * | 2020-06-12 | 2020-12-02 | 竹本油脂株式会社 | Method for manufacturing synthetic fiber treatment agent, synthetic fiber treatment agent, synthetic fiber, and method for manufacturing synthetic fiber |
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| KR950023799A (en) * | 1994-01-26 | 1995-08-18 | 도키와 후미가츠 | Textile emulsion composition |
| JPH10192685A (en) * | 1996-12-27 | 1998-07-28 | Nikka Chem Co Ltd | Nonionic surfactant of low foaming property |
| JP3830322B2 (en) * | 2000-02-04 | 2006-10-04 | 旭化成せんい株式会社 | Polytrimethylene terephthalate partially oriented fiber suitable for false twisting |
| JP4136455B2 (en) * | 2002-04-16 | 2008-08-20 | 松本油脂製薬株式会社 | Oil for friction false twisting of synthetic fibers |
| JP4624913B2 (en) * | 2005-12-01 | 2011-02-02 | 竹本油脂株式会社 | Synthetic fiber treatment agent and synthetic fiber treatment method |
| JP2007321320A (en) * | 2006-06-05 | 2007-12-13 | Teijin Fibers Ltd | Biodegradable polyester fiber for false twist processing |
| JP2012107366A (en) * | 2010-11-19 | 2012-06-07 | Matsumoto Yushi Seiyaku Co Ltd | Friction false twist treatment agent for synthetic fiber and application of the same |
| JP2013155470A (en) * | 2012-01-31 | 2013-08-15 | Nicca Chemical Co Ltd | Scouring agent for fiber and nonionic surfactant |
| CN102875798A (en) * | 2012-10-19 | 2013-01-16 | 大连广汇科技有限公司 | Synthetic method of water insoluble polyether synthetic base oil |
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| 脂肪醇聚醚工业化生产及应用研究;许祥娟;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20121015(第10期);第21-22页第（3）节 * |
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