WO2015166603A1 - Agent for treating short-staple fibers and use for said agent - Google Patents

Agent for treating short-staple fibers and use for said agent Download PDF

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Publication number
WO2015166603A1
WO2015166603A1 PCT/JP2014/080844 JP2014080844W WO2015166603A1 WO 2015166603 A1 WO2015166603 A1 WO 2015166603A1 JP 2014080844 W JP2014080844 W JP 2014080844W WO 2015166603 A1 WO2015166603 A1 WO 2015166603A1
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compound
fiber
weight
treatment agent
group
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PCT/JP2014/080844
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French (fr)
Japanese (ja)
Inventor
充宏 多田
裕志 小南
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松本油脂製薬株式会社
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Priority to CN201480065628.8A priority Critical patent/CN105793486B/en
Publication of WO2015166603A1 publication Critical patent/WO2015166603A1/en

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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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
    • D06M13/165Ethers
    • D06M13/17Polyoxyalkyleneglycol ethers
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244Treating 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 sulfur or phosphorus
    • D06M13/282Treating 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 sulfur or phosphorus with compounds containing phosphorus
    • D06M13/292Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53Polyethers

Definitions

  • the present invention relates to a fiber treatment agent for short fibers and use thereof.
  • the production process of spun yarn includes many spinning processes such as a fiber opening process, a card process, a drawing process, a roving process, a spinning process, and a rewinding process.
  • Synthetic fibers such as polyester, nylon and acrylic, unlike natural fibers such as cotton, do not have oil or fat on the fiber surface, so untreated synthetic fibers lack smoothness and antistatic properties in the spinning process.
  • a fiber treatment agent is generally applied to improve smoothness and antistatic properties.
  • the spinning process has been speeded up from the viewpoint of improving the productivity of spun yarn.
  • the conventional spinning speed is about 100 m / min, but the recent spinning speed is 150 m / min or more.
  • Patent Document 1 The fiber treatment agent described in Patent Document 1 has been recognized to improve spinnability in the card process or the spinning process.
  • the short fiber to which the fiber processing agent for high speed described in Patent Document 1 is applied in the drawing process, if the drawing speed exceeds 500 m / min, coiling failure occurs, and the productivity is lowered.
  • the high-speed fiber treatment agent described in Patent Document 1 has too low friction between the strip sliver and the coiler plate.
  • the objective of this invention is providing the fiber treatment agent for short fibers which is excellent in the coiling property in a high-speed kneading
  • the fiber treatment agent for short fibers contains a specific organophosphate compound and a specific polyoxyalkylene compound in a specific ratio. I found it. That is, the fiber treatment agent for short fibers of the present invention includes a compound (A) represented by the following general formula (1), a compound (B1) represented by the following general formula (2), and the following general formula (3).
  • the weight ratio of the compound (A) to the whole nonvolatile content of the treating agent is 1 to 16% by weight
  • the weight ratio of the compound (D) to the whole nonvolatile content of the treating agent is 25 to 50% by weight
  • the weight ratio of the compound (E) to the entire nonvolatile content of the treating agent is 20 to 40% by weight
  • the weight ratio (A / B) of the compound (A) and the compound (B) is 0.01 to 0.70
  • the weight ratio of inorganic phosphoric acid to the whole nonvolatile content of the treatment agent is 1% by weight or less. .
  • R 1 .Q 2 is a straight-chain alkyl group .
  • Q 1 is hydrogen atom, an alkali metal salt or linear alkyl group having 16 to 18 carbon atoms having 16 to 18 carbon atoms, respectively Independently, a hydrogen atom or an alkali metal salt.
  • R 2 represents an alkyl group, alkenyl group, aryl group or acyl group having 8 to 18 carbon atoms, and may be composed of either a linear or branched structure.
  • PO is an oxypropylene group.
  • EO represents an oxyethylene group
  • a 1 O represents an oxyalkylene group having 2 or 3 carbon atoms
  • a, b and c represent the average number of moles added, a being 0 to 10, and b being 0 to 10
  • C is 1 to 20.
  • [(PO) a / (EO) b ] is a polyoxyalkylene group formed by randomly adding a mole of PO and b mole of EO.)
  • a 2 O is an oxyalkylene group having 2 or 3 carbon atoms
  • m and n are the average number of added moles of the oxyalkylene group
  • m + n is a number from 2 to 20.
  • R 3 is the number of carbon atoms. (8 to 16 alkyl groups, alkenyl groups or aryl groups, each of which may be composed of a linear or branched structure)
  • R 4 is a linear alkyl group having 16 to 18 carbon atoms.
  • R 5 is a linear alkyl group having 16 to 18 carbon atoms.
  • M 1 is a hydrogen atom or an alkali metal salt.
  • R 6 is a linear alkyl group having 16 to 18 carbon atoms.
  • M 2 and M 3 are each independently a hydrogen atom or an alkali metal salt.
  • R 2 is preferably an alkyl group, alkenyl group or aryl group having 8 to 18 carbon atoms.
  • the compound (B) is the compound (B1), and the A 1 O is preferably an oxyethylene group.
  • the moisture absorption rate of the non-volatile content of the treatment agent is preferably 1 to 15% by weight.
  • the a is preferably 1 to 10 and the b is 1 to 10. It is preferable that the weight ratio of the alkyl phosphate ester potassium salt having 6 to 8 carbon atoms in the entire nonvolatile content of the treatment agent is less than 3% by weight.
  • the short fiber of the present invention is one in which the fiber treatment agent is applied to the fiber body.
  • the short fiber to which the fiber treatment agent for short fibers of the present invention is applied is excellent in coiling property at high-speed kneading.
  • the short fiber of the present invention is excellent in productivity since it is excellent in coiling property in high-speed kneading.
  • the schematic diagram explaining the strip evaluation method Schematic drawing explaining the criteria for judging the evaluation of the strips.
  • the fiber treatment agent for short fibers of the present invention essentially contains the compound (A), the compound (B), the compound (D) and the compound (E), and the compound (A) and the compound (B) at a specific ratio. It contains. This will be described in detail below.
  • Compound (A) is an essential component for the present invention.
  • Compound (A) has a solid dry property and is excellent in hygroscopicity. Many of the solids tend to have insufficient convergence, but the compound (A) has excellent hygroscopicity even though it is a solid, and therefore has adequate convergence.
  • the drawing coiling property which is the subject of the present invention, requires low friction between the drawing sliver and the coiler plate, and moderate fiber-fiber friction for maintaining the sliver shape. When a certain amount of the compound (A) is contained in the fiber treatment agent, the fiber to which the treatment agent is applied is excellent in drawing coiling properties.
  • the fiber-fiber friction is too low and the coiling property of the drawing is reduced.
  • the compound (A) is contained in a certain amount, the fiber-fiber friction and Due to the high fiber-metal friction, the coiling property of the drawing is reduced.
  • the compound (A) is excellent in hygroscopicity is not clear, but since it has a structure in which a polar group-containing compound such as water is easily coordinated, it is presumed that it is particularly easy to retain moisture.
  • the reason why the compound (A) is excellent in convergence is not clear, but compared with the monoalkyl phosphate phosphate salt which is the compound (E) described later and the dialkyl phosphate phosphate salt which is the compound (D) described later, the compound (A ) Is large, it is assumed that the intermolecular force for converging the fibers is large.
  • R 1 is a linear alkyl group having 16 to 18 carbon atoms.
  • alkyl group examples include a hexadecyl group, a heptadecyl group, and an octadecyl group, and an octadecyl group is preferable from the viewpoint of strip coiling properties. If R 1 is less than 16, the friction is too low, which is unsuitable from the viewpoint of drawing coiling properties. If R 1 is more than 18, the friction is too high, which is unsuitable from the viewpoint of drawing coiling properties.
  • Q 1 is a hydrogen atom, an alkali metal salt or a linear alkyl group having 16 to 18 carbon atoms.
  • alkali metal salt examples include potassium salt and sodium salt, and potassium salt is preferable from the viewpoint of strip coiling property.
  • Q 2 is a hydrogen atom or an alkali metal salt. Examples of the alkali metal salt include potassium salt and sodium salt, and potassium salt is preferable from the viewpoint of strip coiling property.
  • Compound (A) can be detected as follows. [ 31 P-NMR method] About 30 mg of the measurement sample non-volatile content was weighed into an NMR sample tube having a diameter of 5 mm, dissolved by adding about 0.5 ml of heavy water (D 2 O) as a deuterated solvent, and 31 P-NMR measurement apparatus (manufactured by BRUKER) (AVANCE 400, 162 MHz). The peak of phosphorus element derived from the compound (A) is detected at -5 to -15 ppm.
  • 31 P-NMR method About 30 mg of the measurement sample non-volatile content was weighed into an NMR sample tube having a diameter of 5 mm, dissolved by adding about 0.5 ml of heavy water (D 2 O) as a deuterated solvent, and 31 P-NMR measurement apparatus (manufactured by BRUKER) (AVANCE 400, 162 MHz). The peak of phosphorus element derived from the compound (A) is detected at -5 to -15 ppm
  • Specific examples of the compound (A) represented by the general formula (1) include polystearyl phosphate potassium salt, polystearyl phosphate sodium salt, polycetyl phosphate potassium salt and polycetyl phosphate sodium salt.
  • polystearyl phosphate potassium salt is preferable from the viewpoint of strip coiling property.
  • the compound (B) is an essential component for the present invention. Since the compound (B) has a function of emulsifying the compound (A), the compound (B) is used in combination with the compound (A) at a specific ratio, so that the compound (A) is uniformly applied on the fiber. can do. In addition, since compound (B) has an appropriate fiber-to-fiber friction, it is excellent in drawing coiling properties when used in combination with compound (A) at a specific ratio.
  • Examples of the compound (B) include a compound (B1) described later and a compound (B2) described later.
  • the compound (B1) is represented by the general formula (2).
  • R 2 represents an alkyl group, alkenyl group, aryl group or acyl group having 8 to 18 carbon atoms, and may be composed of either a linear or branched structure.
  • the number of carbon atoms is 8 to 18, preferably 10 to 16, and more preferably 11 to 15 because the fiber-to-fiber friction is moderate and the drawing coiling property is excellent. preferable.
  • the alkyl group may be composed of either a straight chain or branched chain structure, but is preferably a mixture of branched and straight chain from the viewpoint of strip coiling.
  • R 2 is an acyl group
  • the number of carbon atoms is 8 to 18, preferably 10 to 16, and more preferably 11 to 15 because the fiber-fiber friction is moderate and the coiling property is excellent. preferable.
  • PO is an oxypropylene group
  • a represents the average number of moles added of the oxypropylene group.
  • the average added mole number a of the oxypropylene group is 0 to 10, preferably 1 to 10, more preferably 1 to 9, still more preferably 1 to 7, and particularly preferably 2 to 5.
  • the average number of added moles of oxypropylene groups is more than 10, the fiber-metal friction becomes too high, and the coiling property of the drawing is lowered.
  • EO represents an oxyethylene group
  • b represents the average number of added moles of the oxyethylene group.
  • the average added mole number b of the oxyethylene group is 0 to 10, preferably 1 to 10, more preferably 1 to 8, still more preferably 2 to 7, and particularly preferably 3 to 5. If it exceeds 10 moles, the fiber-metal friction becomes too high, and the coiling property of the drawing is lowered.
  • a 1 O is an oxyalkylene group having 2 or 3 carbon atoms, and the average added mole number c of the oxyalkylene group is 1 to 20, preferably 1 to 12. To 8 is more preferable, and 2 to 5 is more preferable.
  • the average addition mole number c of the oxyalkylene group is less than 1, the fiber-metal friction is lowered, and the coiling property of the drawing is lowered.
  • the average addition mole number c of the oxyalkylene group is more than 20, the fiber-metal friction becomes too high, and the coiling property of the drawing is lowered.
  • the A 1 O is an oxyethylene group from the viewpoint of easily obtaining the effect of the present application.
  • the compound (B1) is an alkylene oxide in an alcohol represented by the general formula R 2 OH.
  • the compound (B1) is obtained by randomly adding ethylene oxide and propylene oxide. It can be produced by adding an alkylene oxide. Random addition refers to an addition state in which oxypropylene groups and oxyethylene groups are randomly copolymerized and arranged.
  • R 2 is an acyl group, it is obtained by an ester reaction between a fatty acid represented by the general formula R 2 OH and a corresponding polyalkylene glycol.
  • R 2 when R 2 is an alkyl group, alkenyl group or aryl group, the R 2 OH includes octanol, nonanol, decanol, undecanol, dodecanol, tridecanol, tetradecanol, penta Linear alcohols such as decanol, hexadecanol, heptadecanol, octadecanol; 2-ethylhexanol, 2-propylheptanol, 2-butyloctanol, 2-hexyloctanol, 1-hexylheptanol, isodecanol, iso Branched alkanols such as tridecanol, 3,5,5-trimethylhexanol; octenol, nonenol, decenol, undecenol, dodecenol, tridecenol, tetradecenol, penta Linear
  • alcohols may be used alone or in combination of two or more.
  • Specific examples of alcohol products are not particularly limited.
  • the R 2 OH when R 2 is an acyl group, the R 2 OH includes caprylic acid, pelargonic acid, capric acid, lauric acid, myristic acid, myristoleic acid, pentadecanoic acid, palmitic acid. Acid, palmitoleic acid, isocetyl acid, margaric acid, stearic acid, isostearic acid, oleic acid, elaidic acid, vaccenic acid, linoleic acid, linolenic acid, etc. may be mentioned, and these may be used alone or in combination of two or more Good.
  • the compound (B1) include PO (1) / EO (2) -EO (4) -octyl ether, PO (1) / EO (2) -EO (5) -decyl ether, PO (2) / EO (3) -EO (6) -dodecyl ether, PO (2) / EO (3) -EO (7) -tetradecyl ether, PO (3) / EO (4) -EO (8) -hexadecyl Ether, PO (3) / EO (4) -EO (9) -octadecyl ether, PO (1) / EO (2) -EO (4) -2-ethylhexyl ether, PO (1) / EO (2)- EO (4) -3,5,5-trimethylhexyl ether, PO (1) / EO (2) -EO (5) -2-propylheptyl ether, PO (2) / EO (3) -EO (6) -2-butyloctyl ether, PO (2) / /
  • PO (2) / EO (3) -EO (7) -tetradecyl ether, PO (2) / EO is preferable because the fiber-fiber friction is moderate and the coiling property is excellent.
  • (3) -EO (6) -dodecyl ether, PO (2) / EO (4) -EO (2) -isododecyl ether, PO (2) / EO (4) -EO (2) -isotridecyl ether Is preferred.
  • the EO (10) means polyoxyethylene (10 mol)
  • the PO (2) means polyoxypropylene (2 mol)
  • PO (2) / EO (3) means Mean random addition of polyoxyethylene (3 mol) and polyoxypropylene (2 mol).
  • the PEG (400) means polyethylene glycol (molecular weight 400).
  • the fiber treatment agent of the present invention may contain a compound (B2) (hereinafter sometimes referred to as compound (B2)) which is a polyoxyalkylene alkylamino ether represented by the following general formula (3).
  • the compound (B2) has a function of emulsifying the compound (A) and an antistatic property. It is estimated that the reason why the compound (B2) has an excellent function of emulsifying the compound (A) is that the unshared electron pair of the amino group is coordinated to the hydroxyl group or alkali metal salt of the compound (A). .
  • a 2 O is an oxyalkylene group having 2 or 3 carbon atoms
  • m and n are the average number of added moles of the oxyalkylene group
  • m + n is a number from 2 to 20.
  • R 3 is the number of carbon atoms.
  • examples of R 3 include octyl group, nonyl group, decyl group, undecyl group, dodecyl group, tridecyl group, tetradecyl group, pentadecyl group, and hexadecyl group.
  • One type or two or more types are used in combination. May be.
  • the average added mole number (m + n) of the oxyalkylene group is preferably 2 to 20, more preferably 3 to 18, still more preferably 5 to 15, and particularly preferably 7 to 12. If it exceeds 20, the friction between the fiber and the metal becomes too high, so that the coiling property may be lowered. If it is less than 2, it is difficult to dissolve in water, and the effects of the present application may not be obtained.
  • a 2 O is an oxyalkylene group having 2 or 3 carbon atoms. Random addition of oxyethylene / oxypropylene or block addition may be used. A 2 O is preferably an oxyethylene group from the viewpoint of more exerting the effect of the present application.
  • Compound (D) is a dialkyl phosphate ester and / or a dialkyl phosphate ester salt.
  • the compound (D) has a high fiber-fiber friction, and when the compound (D) is contained in a certain amount in the fiber treatment agent, the treatment agent can impart an appropriate fiber-fiber friction to the fiber. , It will have excellent coiling properties.
  • R 4 is a linear alkyl group having 16 to 18 carbon atoms.
  • R 5 is a linear alkyl group having 16 to 18 carbon atoms.
  • M 1 is a hydrogen atom or an alkali metal salt.
  • R 4 and R 5 are each independently a linear alkyl group having 16 to 18 carbon atoms.
  • the alkyl group include a hexadecyl group, a heptadecyl group, and an octadecyl group, and an octadecyl group is preferable from the viewpoint of strip coiling properties.
  • M 1 is a hydrogen atom or an alkali metal salt.
  • the alkali metal salt include potassium salt and sodium salt, and potassium salt is preferable from the viewpoint of strip coiling property.
  • Compound (D) can be detected by the 31 P-NMR method in the same manner as compound (A).
  • the peak of phosphorus element derived from the compound (D) is detected at +4 to -1 ppm.
  • the peak of phosphorus element derived from compound (D), compound (E) and inorganic phosphoric acid is detected at +4 to ⁇ 1 ppm, but from the low magnetic field side, inorganic phosphoric acid, compound (E), compound (D ) Is determined in the order.
  • Specific examples of the compound (D) represented by the general formula (4) include distearyl phosphate potassium salt, distearyl phosphate sodium salt, dicetyl phosphate potassium salt and dicetyl phosphate sodium salt. Of these, distearyl phosphate ester potassium salt is preferable from the viewpoint of strip coiling properties.
  • Compound (E) is a monoalkyl phosphate ester salt and / or a monoalkyl phosphate ester.
  • Compound (E) has a moderately low fiber-fiber friction and is contained in a certain amount in the fiber treatment agent, so that the treatment agent can impart an appropriate fiber-fiber friction to the fiber. As a result, the drawing coiling property is excellent.
  • R 6 is a linear alkyl group having 16 to 18 carbon atoms.
  • M 2 and M 3 are each independently a hydrogen atom or an alkali metal salt.
  • R 6 is a linear alkyl group having 16 to 18 carbon atoms.
  • the alkyl group include a hexadecyl group, a heptadecyl group, and an octadecyl group, and an octadecyl group is preferable from the viewpoint of strip coiling properties.
  • M 2 and M 3 are each independently a hydrogen atom or an alkali metal salt. Examples of the alkali metal salt include potassium salt and sodium salt, and potassium salt is preferable from the viewpoint of strip coiling property.
  • Specific examples of the compound (E) represented by the general formula (5) include monostearyl phosphate potassium salt, monostearyl phosphate sodium salt, monocetyl phosphate potassium salt and monocetyl phosphate sodium salt.
  • monostearyl phosphate potassium salt is preferable from the viewpoint of strip coiling property.
  • Compound (E) can be detected by the 31 P-NMR method in the same manner as compound (A).
  • the peak of phosphorus element derived from the compound (E) is detected at +4 to -1 ppm.
  • the peak of phosphorus element derived from compound (D), compound (E) and inorganic phosphoric acid is detected at +4 to ⁇ 1 ppm, but from the low magnetic field side, inorganic phosphoric acid, compound (E), compound (D ) Is determined in the order.
  • the fiber treatment agent of the present invention may contain other components in addition to the compound (A), the compound (B), the compound (D), and the compound (E) described above.
  • Other components include, for example, water; other surfactants; antifoaming agents; preservatives; fatty acid alkyl esters, paraffin wax, smoothing agents such as dimethylsilicone components, etc., as long as the effects of the present invention are not impaired. Can do.
  • the fiber treatment agent of the present invention may further contain a smoothing agent.
  • examples of other surfactants include nonionic surfactants other than the compound (B).
  • Nonionic surfactants other than compound (B) include polyhydric alcohol partial ester type nonionic surfactants such as sorbitan trioleate and glycerol monolaurate, polyoxyalkylene sorbitan trioleate, polyoxyalkylene castor oil, polyoxyalkylene Polyoxyalkylene polyhydric alcohol fatty acid ester type nonionic surfactant such as hydrogenated castor oil trioctanoate, alkylamide type nonionic surfactant such as ethanolamine monolauramide, and polyoxyalkylene such as polyoxyethylenediethanolamine monooleylamide Examples include fatty acid amide type nonionic surfactants.
  • the fiber treatment agent of the present invention is preferably an aqueous liquid (emulsion) further containing water in terms of appearance stability and fluidity.
  • the blending ratio of the total amount of the compound (A), the compound (B), the compound (D) and the compound (E) in the entire fiber treatment agent is not particularly limited. However, it is preferably 0.01 to 20% by weight, more preferably 0.02 to 10% by weight, and still more preferably 0.1 to 5% by weight.
  • the blending ratio of the total amount of the compound (A), the compound (B), the compound (D) and the compound (E) in the entire fiber treatment agent is less than 0.01% by weight, desired performance cannot be obtained.
  • a higher liquid content ratio of the weight of the fiber treatment agent to be fed to the fiber weight
  • dripping may increase.
  • it exceeds 20% by weight the stability of the fiber treatment agent becomes poor, precipitation of the compound (A) is likely to occur, and the solution may be thickened.
  • the fiber treatment agent for short fibers of the present invention is a fiber treatment agent for imparting to raw material short fibers to which no treatment agent is imparted.
  • the fiber length of the raw material short fibers is preferably 9 to 64 mm, more preferably 13 to 51 mm, still more preferably 20 to 44 mm, and particularly preferably 31 to 38 mm. If the fiber length is less than 9 mm and more than 64 mm, the high-speed drawing coiling property may be lowered.
  • the thickness of the raw short fiber is generally expressed in units of decitex (hereinafter expressed as dtex), preferably 0.7 to 4.0 dtex, more preferably 0.8 to 3.0 dtex, and 0.0.
  • 9 to 2.0 dtex is more preferable, and 1.0 to 1.5 dtex is particularly preferable. If it is less than 0.7 dtex, the card passing property is lowered, so that the high-speed drawing coiling property may be lowered. If it exceeds 4.0 dtex, the focusing property is lowered, so that the high-speed drawing coiling property may be lowered.
  • the weight ratio of the compound (A) to the whole nonvolatile content of the treatment agent is 1 to 16% by weight, preferably 3 to 15% by weight, and preferably 5 to 14% by weight. More preferably, it is 7 to 13% by weight, further preferably 9 to 12% by weight. If it is less than 1% by weight, the effect of the compound (A) is not exhibited, and the strip coiling property is lowered. If it exceeds 16% by weight, the friction between the coiler plate and the fiber becomes high, so that the coiling property of the drawing is lowered.
  • the non-volatile content in the present invention refers to an absolutely dry component when the treatment agent is heat treated at 105 ° C. to remove the solvent and the like and reach a constant weight.
  • the weight ratio (A / B) of the compound (A) and the compound (B) is 0.01 to 0.7, preferably 0.01 to 0.6, more preferably 0.03 to 0.6. 0.07 to 0.6 is more preferable, 0.1 to 0.5 is particularly preferable, and 0.2 to 0.4 is most preferable. If it is less than 0.01, since the weight of the compound (A) is small, the effect of improving the strip coiling property cannot be obtained. If it exceeds 0.7, emulsification of the compound (A) by the compound (B) becomes insufficient, and the effect of strip coiling property cannot be obtained.
  • the weight ratio of inorganic phosphoric acid to the entire nonvolatile content of the treatment agent is 1% by weight or less, preferably 0.8% by weight or less, and more preferably 0.5% by weight or less. , Less than 0.3% by weight is particularly preferred. A preferred lower limit is 0% by weight. If the inorganic phosphoric acid content exceeds 1% by weight, the affinity with rubber and metal is strong, so that in the drawing process, it adheres to and accumulates on the drawing coiler plate, and the friction between fiber and metal increases rapidly. Coiling performance decreases.
  • Inorganic phosphoric acid can be detected by the 31 P-NMR method as in the case of the compound (A).
  • the peak of phosphorus element derived from inorganic phosphoric acid is detected at +4 to -1 ppm.
  • the peak of phosphorus element derived from compound (D), compound (E) and inorganic phosphoric acid is detected at +4 to ⁇ 1 ppm, but from the low magnetic field side, inorganic phosphoric acid, compound (E), compound (D ) Is determined in the order.
  • the moisture absorption rate of the nonvolatile component of the treatment agent is preferably 1 to 15% by weight, more preferably 2 to 13% by weight, and more preferably 3 to 11% by weight. Further preferred is 4 to 9% by weight.
  • the fiber-to-fiber friction of the spinning treatment agent becomes appropriate, and thus the coiling coiling property is excellent. If the moisture absorption rate is less than 1% by weight, the fiber-to-fiber friction is too low and the effects of the present application may not be exhibited. If it exceeds 15% by weight, the fiber-fiber friction is so high that the effects of the present application may not be exhibited.
  • the moisture absorption rate of the non-volatile content of the treating agent here is measured as follows.
  • the treatment agent occupies the entire nonvolatile content of the treatment agent from the viewpoint that the treatment agent can impart an appropriate fiber-fiber friction to the fiber by being contained in a certain amount in the fiber treatment agent for short fibers of the present invention.
  • the weight ratio of the compound (D) is 25 to 50% by weight, preferably 25 to 45% by weight, and more preferably 30 to 45% by weight.
  • the treatment agent occupies the entire nonvolatile content of the treatment agent from the viewpoint that the treatment agent can impart an appropriate fiber-fiber friction to the fiber by being contained in a certain amount in the fiber treatment agent for short fibers of the present invention.
  • the weight ratio of the compound (E) is 20 to 40% by weight, preferably 25 to 40% by weight, and more preferably 25 to 35% by weight.
  • the weight of each compound in the total weight of the compound (A), the compound (D), the compound (E) and the inorganic phosphoric acid is such that the friction between the fiber and the metal becomes an appropriate value, and from the viewpoint of the preferred strip coiling property, As shown.
  • the weight ratio of the compound (A) is preferably 1 to 25% by weight, more preferably 2 to 25% by weight, based on the total weight of the compound (A), the compound (D), the compound (E) and the inorganic phosphoric acid. It is more preferably 3 to 20% by weight, particularly preferably 4 to 15% by weight, and most preferably 5 to 13% by weight.
  • the weight ratio of the compound (D) is preferably 20 to 60% by weight, more preferably 25 to 55% by weight, based on the total weight of the compound (A), the compound (D), the compound (E) and the inorganic phosphoric acid. It is more preferably 25 to 50% by weight, and further preferably 25 to 45% by weight.
  • the weight ratio of the compound (E) is preferably 10 to 50% by weight, more preferably 15 to 45% by weight, based on the total weight of the compound (A), the compound (D), the compound (E) and the inorganic phosphoric acid. More preferably, it is 20 to 40% by weight.
  • the weight ratio of the inorganic phosphoric acid is preferably 1.0% by weight or less, more preferably 0.5% by weight, based on the total weight of the compound (A), the compound (D), the compound (E) and the inorganic phosphoric acid. More preferably, it is 2% by weight, particularly preferably 0.1% by weight or less.
  • the fiber treatment agent for short fibers of the present invention is used in at least one step selected from a spinning step, a drawing step and a finishing step for producing a synthetic fiber for short fibers.
  • the fiber treatment agent for short fibers of the present invention is preferably used for spinning because the effect of the present invention is easily exhibited.
  • the weight ratio of the alkyl phosphate potassium salt having 6 to 8 carbon atoms in the entire nonvolatile content of the treatment agent is less than 10% by weight from the viewpoint of reducing the coiling property of the drawing. 3 wt% or less is more preferable, 2 wt% or less is more preferable, and 1 wt% or less is particularly preferable. A preferred lower limit is 0% by weight.
  • the fiber treatment agent for short fibers of the present invention is characterized by containing the compound (A) in a specific ratio, and the method for producing the fiber treatment agent for short fibers of the present invention includes a compound at the time of producing the organic phosphate compound.
  • a method of adjusting the content ratio of (A) and then blending the compound (B) and the like can be mentioned.
  • an organic phosphoric acid compound performs the process (I) which makes an organic hydroxyl compound and phosphoric anhydride react, and obtains a reaction material.
  • the ratio of the compound (A) contained in the organic phosphoric acid compound can be adjusted by performing the step (II) of adding water to the reaction product and hydrolyzing it.
  • the amount of water added to the reaction product is preferably 0.01 to 1 mol, more preferably 0.03 to 0.8 mol, and even more preferably 0.05 to 0.5 mol with respect to the organic hydroxyl compound.
  • 0.07 to 0.3 mol is more preferable. If it is less than 0.01 mol and more than 1 mol, it may be difficult to adjust the amount of the compound (A).
  • the fiber treatment agent for short fibers of the present invention comprises a liquid mixture obtained by previously mixing an aqueous liquid containing the compound (A), the compound (D), and the compound (E) with the compound (B) and other components, Manufactured by mixing with other components as required.
  • the compound (A) is composed of other components (specifically, the compound (B) and as necessary. It is preferable not to coexist with at least one selected from other used components to be used.
  • the product stability of the resulting fiber treating agent of the present invention is deteriorated, and appearance defects such as separation and aggregation may occur over time.
  • the product stability of the fiber treatment agent of this invention obtained is favorable, and there is no problem.
  • the short fiber of the present invention is obtained by adding the fiber treatment agent for short fiber of the present invention to the raw short fiber.
  • the application amount of the fiber treatment agent for short fibers is 0.05 to 2.0% by weight, preferably 0.06 to 1.5% by weight, and 0.07 to 1.0% by weight based on the raw short fibers. % Is more preferable, and 0.08 to 0.7% by weight is most preferable. If it is less than 0.05% and more than 2.0% by weight, the card passing property in the spinning process may be inferior.
  • the fiber treatment agent for short fibers of the present invention may be adhered to the raw material short fiber main body without being diluted as it is, and diluted with water to a concentration such that the weight ratio of the entire nonvolatile content becomes 0.01 to 10% by weight. And you may make it adhere to the raw material short fiber main body as an emulsion.
  • the step of adhering the fiber treatment agent for short fibers to the raw material short fiber body may be any of the spinning process, drawing process, crimping process, cutting process and the like of the raw material short fiber body.
  • the means for attaching the fiber treatment agent for short fibers of the present invention to the raw short fiber body is not particularly limited, and means such as roller oil supply, nozzle spray oil supply, and dip oil supply may be used.
  • a method for obtaining the desired adhesion rate more uniformly and efficiently may be adopted in accordance with the short fiber manufacturing process and its characteristics. Moreover, as a drying method, you may use the method of drying with a hot air and infrared rays, the method of making it contact with a heat source, and drying.
  • the raw material short fibers of the present invention include cotton fibers, natural fibers such as bleached cotton fibers, regenerated fibers such as rayon fibers, cupra fibers, acetate fibers, polyolefin fibers, polyester fibers, polyamide fibers, acrylic fibers, polychlorinated fibers.
  • Examples thereof include synthetic fibers such as vinyl fibers and composite fibers composed of two or more kinds of thermoplastic resins.
  • the polyamide fiber include 6-nylon fiber, 6,6-nylon fiber, and aromatic polyamide fiber.
  • rayon fiber examples include viscose rayon fiber, strong rayon fiber, high strength rayon fiber, high wet elastic rayon fiber, solvent-spun rayon fiber, and polynosic fiber.
  • polyolefin resin / polyolefin resin for example, high density polyethylene / polypropylene, linear high density polyethylene / polypropylene, low density polyethylene / polypropylene, two types of propylene and other ⁇ -olefins are used.
  • examples thereof include an original copolymer or a terpolymer / polypropylene, linear high-density polyethylene / high-density polyethylene, and low-density polyethylene / high-density polyethylene.
  • polyolefin resin / polyester resin for example, polypropylene / polyethylene terephthalate, high-density polyethylene / polyethylene terephthalate, linear high-density polyethylene / polyethylene terephthalate, and low-density polyethylene / polyethylene terephthalate.
  • polyester-type resin / polyester-type resin copolymer polyester / polyethylene terephthalate etc. are mentioned, for example.
  • the fiber which consists of polyamide-type resin / polyester-type resin, polyolefin-type resin / polyamide-type resin, etc. is mentioned.
  • the raw material fiber is a polyester fiber
  • the amount of titanium oxide internally added as a matting agent is not suitable, the raw material fiber tends to be deteriorated, particularly, the coiling property tends to be reduced.
  • a fiber is preferable.
  • the weight ratio of the titanium oxide contained in the polyester fiber is preferably 1500 to 4000 ppm, more preferably 1700 to 3500 ppm, and still more preferably 2000 to 3000 ppm from the viewpoint that the effect of the present application is more easily exhibited.
  • the cross-sectional shape of the fiber can be circular or irregular.
  • an irregular shape for example, a flat shape, a polygonal shape such as a triangle to an octagon, a T shape, a hollow shape, a multileaf shape, and the like can be used.
  • the cross-sectional structure of the fiber can be exemplified by a sheath core type, a parallel core type, an eccentric sheath core type, a multilayer type, a radiation type, or a sea island type. Or a parallel type is preferable.
  • the fiber length of the short fiber of the present invention is preferably 9 to 64 mm, more preferably 13 to 51 mm, still more preferably 20 to 44 mm, and particularly preferably 31 to 38 mm. If the fiber length is less than 9 mm and more than 64 mm, the high-speed drawing coiling property may be lowered.
  • the thickness of the short fiber of the present invention is generally expressed in units of decitex (hereinafter expressed as dtex), preferably 0.7 to 4.0 dtex, more preferably 0.8 to 3.0 dtex, 0 Is more preferably 0.9 to 2.0 dtex, and particularly preferably 1.0 to 1.5 dtex. If it is less than 0.7 dtex, the card passing property is lowered, so that the high-speed drawing coiling property may be lowered. If it exceeds 4.0 dtex, the focusing property is lowered, so that the high-speed drawing coiling property may be lowered.
  • the short fiber of the present invention is preferably used for spinning from the viewpoint of easily exerting the effect of the present application
  • compound (E) was 42% by weight with respect to the entire nonvolatile content of the white paste, and inorganic phosphoric acid was 0.1% by weight with respect to the entire nonvolatile content of the white paste. It was done.
  • the phosphoric acid compounds [compound (A), compound (D), and compound (E)] of the above production example described in Table 1, the compound (B1) described in Table 2, the following compound (B2), and compound (F) and the compound (X) were mixed at the ratios shown in Table 3 and stirred to prepare nonvolatile components of the fiber treatment agents for short fibers of each Example and Comparative Example.
  • the non-volatile component was diluted with ion-exchanged water to obtain a 0.5% concentration emulsion.
  • the static electricity amount of the traveling sliver is measured with a Kasuga-type potentiometer at a distance of 1 cm from the traveling sliver 3 cm away from the rubber roller 4 in FIG. Moreover, the above evaluation criteria set ⁇ or more as acceptable. A: Less than 2.0 (kv) (very good) ⁇ : 2.0 or more and less than 10.0 (kv) (good) ⁇ : Over 10 (kv) (defect)
  • the weight ratio of the compound (A) in the entire nonvolatile content of the treatment agent is 1 to 16% by weight
  • the weight ratio of the compound (D) in the total amount is 25 to 50% by weight
  • the weight ratio of the compound (E) in the non-volatile content of the treatment agent is 20 to 40% by weight
  • the compound (A ) And the compound (B) in a weight ratio (A / B) of 0.01 to 0.70 and the amount of inorganic phosphoric acid is 1% by weight or less, the high-speed kneading coiling property was good.
  • Comparative Examples 1 to 5 when the compound (D) and the compound (E) which are phosphoric acid compounds are included but the compound (A) is not included (Comparative Example 1), the compound (A) is the whole non-volatile content of the treating agent.
  • the amount exceeds 30% by weight Comparative Example 2
  • the amount of inorganic phosphoric acid exceeds 1% by weight with respect to the entire nonvolatile content of the treating agent Comparative Example 3
  • the compound (A) is If it is contained but the weight ratio (A / B) of the compound (A) and the previous compound (B) is not in the range of 0.01 to 0.70 (Comparative Example 4), the compound (A) is not contained.
  • the high-speed kneading coiling property was inferior.
  • the treatment agent for short fibers of the present invention can impart high-speed drawing coiling properties to short fibers, the short fibers to which the fiber treatment agent for short fibers of the present invention has been imparted rapidly worldwide. Even if it is spun by a high-speed spinning machine, it is finished into a fine spun yarn with excellent yarn quality.

Abstract

The present invention is an agent for treating short-staple fibers, the agent necessarily containing: a compound (E), a compound (D), and a compound (A) that are specific organophosphoric acid compounds; and a compound (B) that is a specific polyoxyalkylene compound. Said agent contains compounds (A), (D), and (E) in specific ratios. The weight ratio (A/B) of compound (A) and compound (B) is 0.01 to 0.07, and the inorganic phosphoric acid weight ratio is 1% or less. Said agent has exceptional coiling properties under high-speed drawing conditions.

Description

短繊維用繊維処理剤及びその利用Fiber treatment agent for short fibers and use thereof
 本発明は短繊維用繊維処理剤及びその利用に関する。 The present invention relates to a fiber treatment agent for short fibers and use thereof.
 紡績糸の製造工程は、開繊工程、カード工程、練条工程、粗紡工程、精紡工程及び巻き返し工程といった多くの紡績工程を含む。又、ポリエステル、ナイロン及びアクリルのような合成繊維は、コットン等の天然繊維と異なり、繊維表面に油脂が付着していないため、未処理の合成繊維は紡績工程において平滑性や制電性が不足する。従って、一般的に平滑性及び制電性向上のために、繊維処理剤が付与されている。
 近年、紡績糸の生産性向上の観点から、前記紡績工程の高速化が進んでいる。たとえば、カード工程では、従来の紡出速度は100m/min程度であったが、近年の紡出速度は150m/min以上である。また、精紡工程では、従来のスピンドル回転数は16000rpm程度であったが、近年のスピンドル回転数は20000rpm以上である。
 紡績工程の速度向上に伴い、繊維-金属間摩擦及び静電気発生量が高くなるため、紡績各工程の高速化に対応できる短繊維用繊維処理剤の必要性が高まっている。そこで、高速化に対応した繊維処理剤が開発されている(特許文献1)。特許文献1に記載された繊維処理剤は、カード工程又は精紡工程では紡績性の向上が認められてきた。
The production process of spun yarn includes many spinning processes such as a fiber opening process, a card process, a drawing process, a roving process, a spinning process, and a rewinding process. Synthetic fibers such as polyester, nylon and acrylic, unlike natural fibers such as cotton, do not have oil or fat on the fiber surface, so untreated synthetic fibers lack smoothness and antistatic properties in the spinning process. To do. Accordingly, a fiber treatment agent is generally applied to improve smoothness and antistatic properties.
In recent years, the spinning process has been speeded up from the viewpoint of improving the productivity of spun yarn. For example, in the card process, the conventional spinning speed is about 100 m / min, but the recent spinning speed is 150 m / min or more. In the spinning process, the conventional spindle speed is about 16000 rpm, but the spindle speed in recent years is 20000 rpm or more.
As the speed of the spinning process increases, the fiber-metal friction and the amount of static electricity generated increase, so the need for a fiber treatment agent for short fibers that can cope with the speedup of each spinning process is increasing. Therefore, a fiber treatment agent corresponding to high speed has been developed (Patent Document 1). The fiber treatment agent described in Patent Document 1 has been recognized to improve spinnability in the card process or the spinning process.
日本国特開2002-30571号公報Japanese Unexamined Patent Publication No. 2002-30571
 しかし、特許文献1に記載された高速化対応繊維処理剤が付与されてなる短繊維は、練条工程において、練条速度が500m/minを超えるとコイリング性不良が発生し、生産性が低下していた。
 かかるコイリング性不良の原因を調査したところ、特許文献1に記載の高速化対応繊維処理剤は、練条スライバーとコイラープレート間の摩擦が低すぎることが判明した。
 そこで、本発明の目的は、高速練条でのコイリング性に優れる短繊維用繊維処理剤と、該処理剤が付与された短繊維とを提供することである。
However, the short fiber to which the fiber processing agent for high speed described in Patent Document 1 is applied, in the drawing process, if the drawing speed exceeds 500 m / min, coiling failure occurs, and the productivity is lowered. Was.
As a result of investigating the cause of such poor coiling properties, it was found that the high-speed fiber treatment agent described in Patent Document 1 has too low friction between the strip sliver and the coiler plate.
Then, the objective of this invention is providing the fiber treatment agent for short fibers which is excellent in the coiling property in a high-speed kneading | mixing, and the short fiber to which this treatment agent was provided.
 本発明者らは、鋭意検討した結果、特定の有機燐酸化合物と特定のポリオキシアルキレン化合物とを特定の比率で含有する短繊維用繊維処理剤であれば、上記課題を解決することができることを見出した。すなわち、本発明の短繊維用繊維処理剤は、下記一般式(1)で表される化合物(A)と、下記一般式(2)で表される化合物(B1)及び下記一般式(3)で表される化合物(B2)から選ばれる少なくとも1種である化合物(B)と、下記一般式(4)で表される化合物(D)と、下記一般式(5)で表される化合物(E)とを必須に含有し、
処理剤の不揮発分全体に占める前記化合物(A)の重量割合が1~16重量%であり、
処理剤の不揮発分全体に占める前記化合物(D)の重量割合が25~50重量%であり、
処理剤の不揮発分全体に占める前記化合物(E)の重量割合が20~40重量%であり、
前記化合物(A)及び前記化合物(B)の重量比率(A/B)が0.01~0.70であり、処理剤の不揮発分全体に占める無機燐酸の重量割合が1重量%以下である。
As a result of intensive studies, the present inventors have found that the above-described problems can be solved if the fiber treatment agent for short fibers contains a specific organophosphate compound and a specific polyoxyalkylene compound in a specific ratio. I found it. That is, the fiber treatment agent for short fibers of the present invention includes a compound (A) represented by the following general formula (1), a compound (B1) represented by the following general formula (2), and the following general formula (3). A compound (B) that is at least one selected from the compound (B2) represented by the formula (4), a compound (D) represented by the following general formula (4), and a compound represented by the following general formula (5) ( E) and essential
The weight ratio of the compound (A) to the whole nonvolatile content of the treating agent is 1 to 16% by weight,
The weight ratio of the compound (D) to the whole nonvolatile content of the treating agent is 25 to 50% by weight,
The weight ratio of the compound (E) to the entire nonvolatile content of the treating agent is 20 to 40% by weight,
The weight ratio (A / B) of the compound (A) and the compound (B) is 0.01 to 0.70, and the weight ratio of inorganic phosphoric acid to the whole nonvolatile content of the treatment agent is 1% by weight or less. .
Figure JPOXMLDOC01-appb-C000006
Figure JPOXMLDOC01-appb-C000006
(式中、Rは炭素数16~18の直鎖のアルキル基である。Qは水素原子、アルカリ金属塩又は炭素数16~18の直鎖のアルキル基である。Qは、それぞれ独立して、水素原子又はアルカリ金属塩である。) (In the formula, R 1 .Q 2 is a straight-chain alkyl group .Q 1 is hydrogen atom, an alkali metal salt or linear alkyl group having 16 to 18 carbon atoms having 16 to 18 carbon atoms, respectively Independently, a hydrogen atom or an alkali metal salt.)
Figure JPOXMLDOC01-appb-C000007
Figure JPOXMLDOC01-appb-C000007
(式中、Rは炭素数8~18のアルキル基、アルケニル基、アリール基又はアシル基を示し、直鎖又は分枝鎖のいずれの構造から構成されていてもよい。POはオキシプロピレン基、EOはオキシエチレン基、AOは炭素数2又は3のオキシアルキレン基を示す。a、b及びcは、各々の平均付加モル数を示し、aは0~10、bは0~10、cは1~20である。[(PO)/(EO)]はaモルのPOとbモルのEOとがランダム付加してなるポリオキシアルキレン基である。)
Figure JPOXMLDOC01-appb-C000008
(式中、AOは炭素数2又は3のオキシアルキレン基であり、m及びnはオキシアルキレン基の平均付加モル数を示し、m+nは2~20の数である。Rは炭素数8~16のアルキル基、アルケニル基又はアリール基を示し、直鎖又は分枝鎖のいずれの構造から構成されていてもよい。)
(In the formula, R 2 represents an alkyl group, alkenyl group, aryl group or acyl group having 8 to 18 carbon atoms, and may be composed of either a linear or branched structure. PO is an oxypropylene group. , EO represents an oxyethylene group, and A 1 O represents an oxyalkylene group having 2 or 3 carbon atoms, a, b and c represent the average number of moles added, a being 0 to 10, and b being 0 to 10 , C is 1 to 20. [(PO) a / (EO) b ] is a polyoxyalkylene group formed by randomly adding a mole of PO and b mole of EO.)
Figure JPOXMLDOC01-appb-C000008
(In the formula, A 2 O is an oxyalkylene group having 2 or 3 carbon atoms, m and n are the average number of added moles of the oxyalkylene group, and m + n is a number from 2 to 20. R 3 is the number of carbon atoms. (8 to 16 alkyl groups, alkenyl groups or aryl groups, each of which may be composed of a linear or branched structure)
Figure JPOXMLDOC01-appb-C000009
Figure JPOXMLDOC01-appb-C000009
(式中、Rは炭素数16~18の直鎖のアルキル基である。Rは炭素数16~18の直鎖のアルキル基である。Mは水素原子又はアルカリ金属塩である。) (In the formula, R 4 is a linear alkyl group having 16 to 18 carbon atoms. R 5 is a linear alkyl group having 16 to 18 carbon atoms. M 1 is a hydrogen atom or an alkali metal salt. )
Figure JPOXMLDOC01-appb-C000010
Figure JPOXMLDOC01-appb-C000010
(式中、Rは炭素数16~18の直鎖のアルキル基である。MおよびMは、それぞれ独立して、水素原子又はアルカリ金属塩である。) (Wherein R 6 is a linear alkyl group having 16 to 18 carbon atoms. M 2 and M 3 are each independently a hydrogen atom or an alkali metal salt.)
 前記Rは炭素数8~18のアルキル基、アルケニル基又はアリール基であると好ましい。
 前記化合物(B)は前記化合物(B1)であり、前記AOはオキシエチレン基であると好ましい。
 前記処理剤の不揮発分の吸湿率が1~15重量%であると好ましい。
 前記aが1~10及び前記bが1~10であると好ましい。
 処理剤の不揮発分全体に占める炭素数6~8のアルキル燐酸エステルカリウム塩の重量割合が3重量%未満であると好ましい。
R 2 is preferably an alkyl group, alkenyl group or aryl group having 8 to 18 carbon atoms.
The compound (B) is the compound (B1), and the A 1 O is preferably an oxyethylene group.
The moisture absorption rate of the non-volatile content of the treatment agent is preferably 1 to 15% by weight.
The a is preferably 1 to 10 and the b is 1 to 10.
It is preferable that the weight ratio of the alkyl phosphate ester potassium salt having 6 to 8 carbon atoms in the entire nonvolatile content of the treatment agent is less than 3% by weight.
 本発明の短繊維は、前記繊維処理剤が繊維本体に付与されたものである。 The short fiber of the present invention is one in which the fiber treatment agent is applied to the fiber body.
 本発明の短繊維用繊維処理剤を付与した短繊維は、高速練条でのコイリング性に優れる。本発明の短繊維は、高速練条でのコイリング性に優れるため生産性に優れる。 The short fiber to which the fiber treatment agent for short fibers of the present invention is applied is excellent in coiling property at high-speed kneading. The short fiber of the present invention is excellent in productivity since it is excellent in coiling property in high-speed kneading.
練条評価方法を説明する模式図。The schematic diagram explaining the strip evaluation method. 練条評価判断基準を説明する模式図。Schematic drawing explaining the criteria for judging the evaluation of the strips.
 本発明の短繊維用繊維処理剤は、化合物(A)、化合物(B)、化合物(D)及び化合物(E)を必須に含み、化合物(A)と化合物(B)とを特定の比率で含有するものである。以下に詳細に説明する。 The fiber treatment agent for short fibers of the present invention essentially contains the compound (A), the compound (B), the compound (D) and the compound (E), and the compound (A) and the compound (B) at a specific ratio. It contains. This will be described in detail below.
〔化合物(A)〕
 化合物(A)は、本発明に必須の成分である。化合物(A)は、絶乾性状が固体であり、吸湿性に優れる。固体の多くは集束性が不足する傾向にあるが、化合物(A)は、固体であるにも拘わらず吸湿性に優れるため、集束性が適度にある。
 本発明の課題である練条コイリング性は、練条スライバーとコイラープレートとの摩擦が低く、且つ、スライバー形状の維持のための繊維-繊維間摩擦が適度でなければならない。化合物(A)が繊維処理剤中に一定量含まれると、当該処理剤が付与された繊維は、練条コイリング性に優れる。化合物(A)が全く含まれない場合には、繊維-繊維間摩擦が低すぎて練条コイリング性が低下し、化合物(A)が一定量超含まれる場合には、繊維-繊維間摩擦及び繊維-金属間摩擦が高いために、練条コイリング性が低下する。
[Compound (A)]
The compound (A) is an essential component for the present invention. Compound (A) has a solid dry property and is excellent in hygroscopicity. Many of the solids tend to have insufficient convergence, but the compound (A) has excellent hygroscopicity even though it is a solid, and therefore has adequate convergence.
The drawing coiling property, which is the subject of the present invention, requires low friction between the drawing sliver and the coiler plate, and moderate fiber-fiber friction for maintaining the sliver shape. When a certain amount of the compound (A) is contained in the fiber treatment agent, the fiber to which the treatment agent is applied is excellent in drawing coiling properties. When the compound (A) is not contained at all, the fiber-fiber friction is too low and the coiling property of the drawing is reduced. When the compound (A) is contained in a certain amount, the fiber-fiber friction and Due to the high fiber-metal friction, the coiling property of the drawing is reduced.
 化合物(A)が吸湿性に優れる理由としては定かではないが、水等の極性基含有化合物を配位し易い構造を有するため、特に水分を保持し易いものと推定している。
 化合物(A)が集束性に優れる理由は定かではないが、後述する化合物(E)であるモノアルキル燐酸ホスフェート塩及び後述する化合物(D)であるジアルキル燐酸ホスフェート塩と比較して、化合物(A)の分子量が大きいため、繊維-繊維を集束する分子間力が大きいことによるものと推定している。
The reason why the compound (A) is excellent in hygroscopicity is not clear, but since it has a structure in which a polar group-containing compound such as water is easily coordinated, it is presumed that it is particularly easy to retain moisture.
The reason why the compound (A) is excellent in convergence is not clear, but compared with the monoalkyl phosphate phosphate salt which is the compound (E) described later and the dialkyl phosphate phosphate salt which is the compound (D) described later, the compound (A ) Is large, it is assumed that the intermolecular force for converging the fibers is large.
 化合物(A)は、上記一般式(1)で表される。
 一般式(1)中、Rは炭素数16~18の直鎖のアルキル基である。当該アルキル基としては、ヘキサデシル基、ヘプタデシル基、オクタデシル基が挙げられ、練条コイリング性の観点からオクタデシル基が好ましい。Rが16未満では、摩擦が低すぎるために練条コイリング性の観点から不適である。Rが18超では、摩擦が高すぎるために練条コイリング性の観点から不適である。
 一般式(1)中、Qは水素原子、アルカリ金属塩又は炭素数16~18の直鎖のアルキル基である。アルカリ金属塩としては、カリウム塩、ナトリウム塩が挙げられ、カリウム塩が練条コイリング性の観点から好ましい。
 一般式(1)中、Qは水素原子又はアルカリ金属塩である。アルカリ金属塩としては、カリウム塩、ナトリウム塩が挙げられ、カリウム塩が練条コイリング性の観点から好ましい。
The compound (A) is represented by the general formula (1).
In the general formula (1), R 1 is a linear alkyl group having 16 to 18 carbon atoms. Examples of the alkyl group include a hexadecyl group, a heptadecyl group, and an octadecyl group, and an octadecyl group is preferable from the viewpoint of strip coiling properties. If R 1 is less than 16, the friction is too low, which is unsuitable from the viewpoint of drawing coiling properties. If R 1 is more than 18, the friction is too high, which is unsuitable from the viewpoint of drawing coiling properties.
In the general formula (1), Q 1 is a hydrogen atom, an alkali metal salt or a linear alkyl group having 16 to 18 carbon atoms. Examples of the alkali metal salt include potassium salt and sodium salt, and potassium salt is preferable from the viewpoint of strip coiling property.
In general formula (1), Q 2 is a hydrogen atom or an alkali metal salt. Examples of the alkali metal salt include potassium salt and sodium salt, and potassium salt is preferable from the viewpoint of strip coiling property.
 化合物(A)は、次のようにして検出することができる。
31P-NMR法〕
 測定試料不揮発分約30mgを直径5mmのNMR用試料管に秤量し、重水素化溶媒として約0.5mlの重水(DO)を加え溶解させて、31P-NMR測定装置(BRUKER社製AVANCE400,162MHz)で測定した。
 化合物(A)に由来する燐元素のピークは、-5~-15ppmにて検出される。
Compound (A) can be detected as follows.
[ 31 P-NMR method]
About 30 mg of the measurement sample non-volatile content was weighed into an NMR sample tube having a diameter of 5 mm, dissolved by adding about 0.5 ml of heavy water (D 2 O) as a deuterated solvent, and 31 P-NMR measurement apparatus (manufactured by BRUKER) (AVANCE 400, 162 MHz).
The peak of phosphorus element derived from the compound (A) is detected at -5 to -15 ppm.
 一般式(1)で表される化合物(A)の具体例としては、ポリステアリル燐酸エステルカリウム塩、ポリステアリル燐酸エステルナトリウム塩、ポリセチル燐酸エステルカリウム塩及びポリセチル燐酸エステルナトリウム塩等が挙げられる。これらの中でも、練条コイリング性の観点から、ポリステアリル燐酸エステルカリウム塩が好ましい。 Specific examples of the compound (A) represented by the general formula (1) include polystearyl phosphate potassium salt, polystearyl phosphate sodium salt, polycetyl phosphate potassium salt and polycetyl phosphate sodium salt. Among these, polystearyl phosphate potassium salt is preferable from the viewpoint of strip coiling property.
〔化合物(B)〕
 化合物(B)は、本発明に必須の成分である。化合物(B)は、化合物(A)を乳化する機能を有するため、化合物(B)は、化合物(A)と特定の比率で併用使用することで、化合物(A)を繊維上に均一に付与することができる。
 また、化合物(B)は適度な繊維-繊維間摩擦を有するため、化合物(A)と特定の比率で併用使用することで、練条コイリング性に優れる。
[Compound (B)]
The compound (B) is an essential component for the present invention. Since the compound (B) has a function of emulsifying the compound (A), the compound (B) is used in combination with the compound (A) at a specific ratio, so that the compound (A) is uniformly applied on the fiber. can do.
In addition, since compound (B) has an appropriate fiber-to-fiber friction, it is excellent in drawing coiling properties when used in combination with compound (A) at a specific ratio.
 化合物(B)として、後述する化合物(B1)及び後述する化合物(B2)を挙げることができる。
 化合物(B1)は、上記一般式(2)で表される。
 上記一般式(2)式中、Rは炭素数8~18のアルキル基、アルケニル基、アリール基又はアシル基を示し、直鎖又は分枝鎖のいずれの構造から構成されていてもよい。
 Rがアルキル基である場合には、繊維-繊維間摩擦が適度であり、練条コイリング性が優れる理由から、炭素数は8~18であり、10~16が好ましく、11~15がより好ましい。
 当該アルキル基は直鎖又は分枝鎖のいずれの構造から構成されていてもよいが、練条コイリング性の観点から、分岐及び直鎖の混合であることが好ましい。
 Rがアシル基である場合には、繊維-繊維間摩擦が適度であり、練条コイリング性が優れる理由から、炭素数は8~18であり、10~16が好ましく、11~15がより好ましい。
Examples of the compound (B) include a compound (B1) described later and a compound (B2) described later.
The compound (B1) is represented by the general formula (2).
In the general formula (2), R 2 represents an alkyl group, alkenyl group, aryl group or acyl group having 8 to 18 carbon atoms, and may be composed of either a linear or branched structure.
In the case where R 2 is an alkyl group, the number of carbon atoms is 8 to 18, preferably 10 to 16, and more preferably 11 to 15 because the fiber-to-fiber friction is moderate and the drawing coiling property is excellent. preferable.
The alkyl group may be composed of either a straight chain or branched chain structure, but is preferably a mixture of branched and straight chain from the viewpoint of strip coiling.
When R 2 is an acyl group, the number of carbon atoms is 8 to 18, preferably 10 to 16, and more preferably 11 to 15 because the fiber-fiber friction is moderate and the coiling property is excellent. preferable.
 上記一般式(2)式中、POはオキシプロピレン基であり、aはオキシプロピレン基の平均付加モル数を表す。オキシプロピレン基の平均付加モル数aとしては、0~10であり、1~10が好ましく、1~9がより好ましく、1~7が更に好ましく、2~5が特に好ましい。オキシプロピレン基の平均付加モル数が10超であると、繊維-金属間摩擦が高くなり過ぎるため、練条コイリング性が低下する。 In the general formula (2), PO is an oxypropylene group, and a represents the average number of moles added of the oxypropylene group. The average added mole number a of the oxypropylene group is 0 to 10, preferably 1 to 10, more preferably 1 to 9, still more preferably 1 to 7, and particularly preferably 2 to 5. When the average number of added moles of oxypropylene groups is more than 10, the fiber-metal friction becomes too high, and the coiling property of the drawing is lowered.
 上記一般式(2)式中、EOはオキシエチレン基であり、bはオキシエチレン基の平均付加モル数を示す。オキシエチレン基の平均付加モル数bとしては、0~10であり、1~10が好ましく、1~8がより好ましく、2~7が更に好ましく、3~5が特に好ましい。10モルを超えると、繊維-金属間摩擦が高くなり過ぎるため、練条コイリング性が低下する。 In the general formula (2), EO represents an oxyethylene group, and b represents the average number of added moles of the oxyethylene group. The average added mole number b of the oxyethylene group is 0 to 10, preferably 1 to 10, more preferably 1 to 8, still more preferably 2 to 7, and particularly preferably 3 to 5. If it exceeds 10 moles, the fiber-metal friction becomes too high, and the coiling property of the drawing is lowered.
 上記一般式(2)式中、AOは炭素数2又は3のオキシアルキレン基であり、オキシアルキレン基の平均付加モル数cとしては、1~20であり、1~12が好ましく、1~8がより好ましく、2~5がさらに好ましい。オキシアルキレン基の平均付加モル数cが1未満では、繊維-金属間摩擦が低くなるために、練条コイリング性が低下する。オキシアルキレン基の平均付加モル数cが20超では、繊維-金属間摩擦が高くなり過ぎるため、練条コイリング性が低下する。上記一般式(2)式中、上記AOがオキシエチレン基であると、本願効果が得られやすい観点から好ましい。 In the general formula (2), A 1 O is an oxyalkylene group having 2 or 3 carbon atoms, and the average added mole number c of the oxyalkylene group is 1 to 20, preferably 1 to 12. To 8 is more preferable, and 2 to 5 is more preferable. When the average addition mole number c of the oxyalkylene group is less than 1, the fiber-metal friction is lowered, and the coiling property of the drawing is lowered. When the average addition mole number c of the oxyalkylene group is more than 20, the fiber-metal friction becomes too high, and the coiling property of the drawing is lowered. In the general formula (2), it is preferable that the A 1 O is an oxyethylene group from the viewpoint of easily obtaining the effect of the present application.
 一般式(2)中、Rがアルキル基、アルケニル基又はアリール基であり、a=0かつb=0の場合、化合物(B1)は、一般式ROHで表されるアルコールにアルキレンオキサイドを付加させることで得られる。
 一般式(2)中、Rがアルキル基、アルケニル基又はアリール基であり、a=1以上かつb=1以上の場合、化合物(B1)は、エチレンオキサイド及びプロピレンオキサイドをランダム付加させた後、アルキレンオキサイド付加させて製造することができる。ランダム付加とは、オキシプロピレン基およびオキシエチレン基が無秩序に共重合して配列された付加状態になっていることを言う。
 一般式(2)中、Rがアシル基である場合には、一般式ROHで表される脂肪酸と、対応するポリアルキレングリコールとのエステル反応により得られる。
In the general formula (2), when R 2 is an alkyl group, an alkenyl group, or an aryl group, and a = 0 and b = 0, the compound (B1) is an alkylene oxide in an alcohol represented by the general formula R 2 OH. Can be obtained by adding
In the general formula (2), when R 2 is an alkyl group, an alkenyl group or an aryl group, and a = 1 or more and b = 1 or more, the compound (B1) is obtained by randomly adding ethylene oxide and propylene oxide. It can be produced by adding an alkylene oxide. Random addition refers to an addition state in which oxypropylene groups and oxyethylene groups are randomly copolymerized and arranged.
In the general formula (2), when R 2 is an acyl group, it is obtained by an ester reaction between a fatty acid represented by the general formula R 2 OH and a corresponding polyalkylene glycol.
 上記一般式(2)式中、Rがアルキル基、アルケニル基又はアリール基である場合には、上記ROHとしては、オクタノール、ノナノール、デカノール、ウンデカノール、ドデカノール、トリデカノール、テトラデカノール、ペンタデカノール、ヘキサデカノール、ヘプタデカノール、オクタデカノール等の直鎖アルコール;2-エチルヘキサノール、2-プロピルヘプタノール、2-ブチルオクタノール、2-ヘキシルオクタノール、1-ヘキシルヘプタノール、イソデカノール、イソトリデカノール、3,5,5-トリメチルヘキサノール等の分岐アルカノール;オクテノール、ノネノール、デセノール、ウンデセノール、ドデセノール、トリデセノール、テトラデセノール、ペンタデセノール、ヘキサデセノール、ヘプタデセノール、オクタデセノール等の直鎖アルケノール;オクチルフェノール、ノニルフェノール等のアルキルフェノールが挙げられる。これらのアルコールは、1種又は2種以上を併用してもよい。アルコール製品の具体例としては、特に限定はないが、例えば、ヤシアルコール、パームアルコール等の天然油脂由来の高級アルコールや、カルコールシリーズ(花王製)、コノールシリーズ(新日本理化製)、オキソコールシリーズ(協和発酵ケミカル製)、ネオドールシリーズ(シェル化学製)、SAFOLシリーズ(Sasol製)、ALFOLシリーズ(Sasol製)、EXXALシリーズ(エクソン・モービル製)等が挙げられる。これら高級アルコール製品は、1種又は2種以上を併用してもよい。
 上記一般式(2)式中、Rがアシル基である場合には、上記ROHとしては、カプリル酸、ペラルゴン酸、カプリン酸、ラウリン酸、ミリスチン酸、ミリストレイン酸、ペンタデカン酸、パルミチン酸、パルミトレイン酸、イソセチル酸、マルガリン酸、ステアリン酸、イソステアリン酸、オレイン酸、エライジン酸、バクセン酸、リノール酸、リノレン酸等が挙げられ、これらは、1種又は2種以上を併用してもよい。
In the general formula (2), when R 2 is an alkyl group, alkenyl group or aryl group, the R 2 OH includes octanol, nonanol, decanol, undecanol, dodecanol, tridecanol, tetradecanol, penta Linear alcohols such as decanol, hexadecanol, heptadecanol, octadecanol; 2-ethylhexanol, 2-propylheptanol, 2-butyloctanol, 2-hexyloctanol, 1-hexylheptanol, isodecanol, iso Branched alkanols such as tridecanol, 3,5,5-trimethylhexanol; octenol, nonenol, decenol, undecenol, dodecenol, tridecenol, tetradecenol, pentadecenol, hexadecenol, heptadeceno Le, linear alkenol such octadecenol; octylphenol include nonylphenol, and the like. These alcohols may be used alone or in combination of two or more. Specific examples of alcohol products are not particularly limited. For example, higher alcohols derived from natural fats and oils such as coconut alcohol and palm alcohol, the calcoal series (made by Kao), the conol series (made by Shin Nippon Rika), oxo Examples include the Cole series (manufactured by Kyowa Hakko Chemical), the Neodoll series (manufactured by Shell Chemical), the SAFOL series (manufactured by Sasol), the ALFOL series (manufactured by Sasol), the EXXAL series (manufactured by Exxon Mobil). These higher alcohol products may be used alone or in combination of two or more.
In the general formula (2), when R 2 is an acyl group, the R 2 OH includes caprylic acid, pelargonic acid, capric acid, lauric acid, myristic acid, myristoleic acid, pentadecanoic acid, palmitic acid. Acid, palmitoleic acid, isocetyl acid, margaric acid, stearic acid, isostearic acid, oleic acid, elaidic acid, vaccenic acid, linoleic acid, linolenic acid, etc. may be mentioned, and these may be used alone or in combination of two or more Good.
 化合物(B1)の具体例としては、PO(1)/EO(2)-EO(4)-オクチルエーテル、PO(1)/EO(2)-EO(5)-デシルエーテル、PO(2)/EO(3)-EO(6)-ドデシルエーテル、PO(2)/EO(3)-EO(7)-テトラデシルエーテル、PO(3)/EO(4)-EO(8)-ヘキサデシルエーテル、PO(3)/EO(4)-EO(9)-オクタデシルエーテル、PO(1)/EO(2)-EO(4)-2-エチルヘキシルエーテル、PO(1)/EO(2)-EO(4)-3,5,5-トリメチルヘキシルエーテル、PO(1)/EO(2)-EO(5)-2-プロピルヘプチルエーテル、PO(2)/EO(3)-EO(6)-2-ブチルオクチルエーテル、PO(2)/EO(3)-EO(7)-2-ヘキシルオクチルエーテル、PO(2)/EO(4)-EO(2)-イソドデシルエーテル、PO(2)/EO(4)-EO(2)-イソトリデシルエーテル、PO(3)/EO(3)-EO(6)-イソセチルエーテル、PO(3)/EO(3)-EO(6)-イソステアリルエーテル、PO(10)/EO(10)-EO(20)-オクチルエーテル、PO(10)/EO(10)-EO(20)-ドデシルエーテル、PO(10)/EO(10)-EO(20)-ヘキサデシルエーテル、EO(5)-オクチルエーテル、EO(7)-デシルエーテル、EO(10)-ドデシルエーテル、EO(15)-テトラデシルエーテル、EO(20)-ヘキサデシルエーテル、EO(10)-ノニルフェニルエーテル、EO(10)オレイルエーテル、EO(8)ステアリルエーテル、PEG(400)モノラウレート、PEG(600)モノラウレート、PEG(600)モノオレエート等が挙げられ、1種類又は2種以上を併用してもよい。中でも、繊維-繊維間摩擦が適度であるために、練条コイリング性が優れるとの理由から、PO(2)/EO(3)-EO(7)-テトラデシルエーテル、PO(2)/EO(3)-EO(6)-ドデシルエーテル、PO(2)/EO(4)-EO(2)-イソドデシルエーテル、PO(2)/EO(4)-EO(2)-イソトリデシルエーテルが好ましい。
 なお、上記EO(10)は、ポリオキシエチレン(10モル)を意味し、上記PO(2)は、ポリオキシプロピレン(2モル)を意味し、上記PO(2)/EO(3)は、ポリオキシエチレン(3モル)及びポリオキシプロピレン(2モル)のランダム付加を意味する。
上記PEG(400)は、ポリエチレングリコール(分子量400)を意味する。
Specific examples of the compound (B1) include PO (1) / EO (2) -EO (4) -octyl ether, PO (1) / EO (2) -EO (5) -decyl ether, PO (2) / EO (3) -EO (6) -dodecyl ether, PO (2) / EO (3) -EO (7) -tetradecyl ether, PO (3) / EO (4) -EO (8) -hexadecyl Ether, PO (3) / EO (4) -EO (9) -octadecyl ether, PO (1) / EO (2) -EO (4) -2-ethylhexyl ether, PO (1) / EO (2)- EO (4) -3,5,5-trimethylhexyl ether, PO (1) / EO (2) -EO (5) -2-propylheptyl ether, PO (2) / EO (3) -EO (6) -2-butyloctyl ether, PO (2) / EO (3) -EO ( ) -2-hexyloctyl ether, PO (2) / EO (4) -EO (2) -isododecyl ether, PO (2) / EO (4) -EO (2) -isotridecyl ether, PO (3 ) / EO (3) -EO (6) -isocetyl ether, PO (3) / EO (3) -EO (6) -isostearyl ether, PO (10) / EO (10) -EO (20)- Octyl ether, PO (10) / EO (10) -EO (20) -dodecyl ether, PO (10) / EO (10) -EO (20) -hexadecyl ether, EO (5) -octyl ether, EO ( 7) -decyl ether, EO (10) -dodecyl ether, EO (15) -tetradecyl ether, EO (20) -hexadecyl ether, EO (10) -nonylphenyl ether, EO (10) Rail ether, EO (8) stearyl ether, PEG (400) monolaurate, PEG (600) monolaurate, PEG (600) monooleate and the like, may be used alone or one or two. Among them, PO (2) / EO (3) -EO (7) -tetradecyl ether, PO (2) / EO is preferable because the fiber-fiber friction is moderate and the coiling property is excellent. (3) -EO (6) -dodecyl ether, PO (2) / EO (4) -EO (2) -isododecyl ether, PO (2) / EO (4) -EO (2) -isotridecyl ether Is preferred.
The EO (10) means polyoxyethylene (10 mol), the PO (2) means polyoxypropylene (2 mol), and the PO (2) / EO (3) means Mean random addition of polyoxyethylene (3 mol) and polyoxypropylene (2 mol).
The PEG (400) means polyethylene glycol (molecular weight 400).
〔ポリオキシアルキレンアルキルアミノエーテル(B2)〕
 本発明の繊維処理剤は、次の一般式(3)で表されるポリオキシアルキレンアルキルアミノエーテルである化合物(B2)(以後、化合物(B2)ということがある。)を含有してもよい。化合物(B2)は、化合物(A)を乳化する機能及び制電性を有する。化合物(B2)が化合物(A)を乳化する機能が優れる理由としては、アミノ基の非共有電子対が、化合物(A)の水酸基やアルカリ金属塩に配位することによるものと推定している。
[Polyoxyalkylene alkylamino ether (B2)]
The fiber treatment agent of the present invention may contain a compound (B2) (hereinafter sometimes referred to as compound (B2)) which is a polyoxyalkylene alkylamino ether represented by the following general formula (3). . The compound (B2) has a function of emulsifying the compound (A) and an antistatic property. It is estimated that the reason why the compound (B2) has an excellent function of emulsifying the compound (A) is that the unshared electron pair of the amino group is coordinated to the hydroxyl group or alkali metal salt of the compound (A). .
Figure JPOXMLDOC01-appb-C000011
Figure JPOXMLDOC01-appb-C000011
(式中、AOは炭素数2又は3のオキシアルキレン基であり、m及びnはオキシアルキレン基の平均付加モル数を示し、m+nは2~20の数である。Rは炭素数8~16のアルキル基、アルケニル基又はアリール基を示し、直鎖又は分枝鎖のいずれの構造から構成されていてもよい。) (In the formula, A 2 O is an oxyalkylene group having 2 or 3 carbon atoms, m and n are the average number of added moles of the oxyalkylene group, and m + n is a number from 2 to 20. R 3 is the number of carbon atoms. (8 to 16 alkyl groups, alkenyl groups or aryl groups, each of which may be composed of a linear or branched structure)
 一般式(3)中、Rとしては、オクチル基、ノニル基、デシル基、ウンデシル基、ドデシル基、トリデシル基、テトラデシル基、ペンタデシル基、ヘキサデシル基が挙げられ、1種類又は2種以上を併用してもよい。 In general formula (3), examples of R 3 include octyl group, nonyl group, decyl group, undecyl group, dodecyl group, tridecyl group, tetradecyl group, pentadecyl group, and hexadecyl group. One type or two or more types are used in combination. May be.
 一般式(3)中、オキシアルキレン基の平均付加モル数(m+n)としては、2~20が好ましく、3~18がより好ましく、5~15が更に好ましく、7~12が特に好ましい。20を超えると繊維-金属間摩擦が高くなり過ぎるため、コイリング性が低下する可能性がある。2未満では、水に溶解し難く、本願の効果が得られない可能性がある。 In the general formula (3), the average added mole number (m + n) of the oxyalkylene group is preferably 2 to 20, more preferably 3 to 18, still more preferably 5 to 15, and particularly preferably 7 to 12. If it exceeds 20, the friction between the fiber and the metal becomes too high, so that the coiling property may be lowered. If it is less than 2, it is difficult to dissolve in water, and the effects of the present application may not be obtained.
 一般式(3)中、AOは炭素数2又は3のオキシアルキレン基である。オキシエチレン/オキシプロピレンのランダム付加であってもよく、ブロック付加であってもよい。AOは、本願効果をより発揮する観点から、オキシエチレン基が好ましい。 In the general formula (3), A 2 O is an oxyalkylene group having 2 or 3 carbon atoms. Random addition of oxyethylene / oxypropylene or block addition may be used. A 2 O is preferably an oxyethylene group from the viewpoint of more exerting the effect of the present application.
〔化合物(D)〕
 化合物(D)は、ジアルキル燐酸エステル及び/又はジアルキル燐酸エステル塩である。
 化合物(D)は、繊維-繊維間摩擦が高く、繊維処理剤中に一定量含有されることで、処理剤が繊維に対して適度な繊維-繊維間摩擦を付与することができ、その結果、練条コイリング性が優れるものとなる。
[Compound (D)]
Compound (D) is a dialkyl phosphate ester and / or a dialkyl phosphate ester salt.
The compound (D) has a high fiber-fiber friction, and when the compound (D) is contained in a certain amount in the fiber treatment agent, the treatment agent can impart an appropriate fiber-fiber friction to the fiber. , It will have excellent coiling properties.
Figure JPOXMLDOC01-appb-C000012
Figure JPOXMLDOC01-appb-C000012
(式中、Rは炭素数16~18の直鎖のアルキル基である。Rは炭素数16~18の直鎖のアルキル基である。Mは水素原子又はアルカリ金属塩である。) (In the formula, R 4 is a linear alkyl group having 16 to 18 carbon atoms. R 5 is a linear alkyl group having 16 to 18 carbon atoms. M 1 is a hydrogen atom or an alkali metal salt. )
 一般式(4)中、R及びRは、それぞれ独立して、炭素数16~18の直鎖のアルキル基である。当該アルキル基としては、ヘキサデシル基、ヘプタデシル基、オクタデシル基が挙げられ、練条コイリング性の観点からオクタデシル基が好ましい。
 一般式(4)中、Mは水素原子又はアルカリ金属塩である。アルカリ金属塩としては、カリウム塩、ナトリウム塩が挙げられ、カリウム塩が練条コイリング性の観点から好ましい。
In the general formula (4), R 4 and R 5 are each independently a linear alkyl group having 16 to 18 carbon atoms. Examples of the alkyl group include a hexadecyl group, a heptadecyl group, and an octadecyl group, and an octadecyl group is preferable from the viewpoint of strip coiling properties.
In General Formula (4), M 1 is a hydrogen atom or an alkali metal salt. Examples of the alkali metal salt include potassium salt and sodium salt, and potassium salt is preferable from the viewpoint of strip coiling property.
 化合物(D)は、化合物(A)と同様に、31P-NMRの方法で検出することができる。
 化合物(D)に由来する燐元素のピークは、+4~-1ppmにて検出される。化合物(D)、化合物(E)及び無機燐酸に由来する燐元素のピークは、いずれも+4~-1ppmにて検出されるが、低磁場側から、無機燐酸、化合物(E)、化合物(D)の順に帰属が決定される。
Compound (D) can be detected by the 31 P-NMR method in the same manner as compound (A).
The peak of phosphorus element derived from the compound (D) is detected at +4 to -1 ppm. The peak of phosphorus element derived from compound (D), compound (E) and inorganic phosphoric acid is detected at +4 to −1 ppm, but from the low magnetic field side, inorganic phosphoric acid, compound (E), compound (D ) Is determined in the order.
 一般式(4)で表される化合物(D)の具体例としては、ジステアリル燐酸エステルカリウム塩、ジステアリル燐酸エステルナトリウム塩、ジセチル燐酸エステルカリウム塩及びジセチル燐酸エステルナトリウム塩等が挙げられる。これらの中でも、練条コイリング性の観点から、ジステアリル燐酸エステルカリウム塩が好ましい。 Specific examples of the compound (D) represented by the general formula (4) include distearyl phosphate potassium salt, distearyl phosphate sodium salt, dicetyl phosphate potassium salt and dicetyl phosphate sodium salt. Of these, distearyl phosphate ester potassium salt is preferable from the viewpoint of strip coiling properties.
〔化合物(E)〕
 化合物(E)は、モノアルキル燐酸エステル塩及び/又はモノアルキル燐酸エステルである。化合物(E)は、繊維-繊維間摩擦が適度に低く、繊維処理剤中に一定量含有されることで、処理剤が繊維に対して適度な繊維-繊維間摩擦を付与することができ、その結果、練条コイリング性が優れるものとなる。
[Compound (E)]
Compound (E) is a monoalkyl phosphate ester salt and / or a monoalkyl phosphate ester. Compound (E) has a moderately low fiber-fiber friction and is contained in a certain amount in the fiber treatment agent, so that the treatment agent can impart an appropriate fiber-fiber friction to the fiber. As a result, the drawing coiling property is excellent.
Figure JPOXMLDOC01-appb-C000013
Figure JPOXMLDOC01-appb-C000013
(式中、Rは炭素数16~18の直鎖のアルキル基である。MおよびMは、それぞれ独立して、水素原子又はアルカリ金属塩である。) (Wherein R 6 is a linear alkyl group having 16 to 18 carbon atoms. M 2 and M 3 are each independently a hydrogen atom or an alkali metal salt.)
 一般式(5)中、Rは炭素数16~18の直鎖のアルキル基である。当該アルキル基としては、ヘキサデシル基、ヘプタデシル基、オクタデシル基が挙げられ、練条コイリング性の観点からオクタデシル基が好ましい。
 一般式(5)中、MおよびMは、それぞれ独立して、水素原子又はアルカリ金属塩である。アルカリ金属塩としては、カリウム塩、ナトリウム塩が挙げられ、カリウム塩が練条コイリング性の観点から好ましい。
In general formula (5), R 6 is a linear alkyl group having 16 to 18 carbon atoms. Examples of the alkyl group include a hexadecyl group, a heptadecyl group, and an octadecyl group, and an octadecyl group is preferable from the viewpoint of strip coiling properties.
In General Formula (5), M 2 and M 3 are each independently a hydrogen atom or an alkali metal salt. Examples of the alkali metal salt include potassium salt and sodium salt, and potassium salt is preferable from the viewpoint of strip coiling property.
 一般式(5)で表される化合物(E)の具体例としては、モノステアリル燐酸エステルカリウム塩、モノステアリル燐酸エステルナトリウム塩、モノセチル燐酸エステルカリウム塩及びモノセチル燐酸エステルナトリウム塩等が挙げられる。これらの中でも、練条コイリング性の観点から、モノステアリル燐酸エステルカリウム塩が好ましい。 Specific examples of the compound (E) represented by the general formula (5) include monostearyl phosphate potassium salt, monostearyl phosphate sodium salt, monocetyl phosphate potassium salt and monocetyl phosphate sodium salt. Among these, monostearyl phosphate potassium salt is preferable from the viewpoint of strip coiling property.
 化合物(E)は、化合物(A)と同様に、31P-NMRの方法で検出することができる。
 化合物(E)に由来する燐元素のピークは、+4~-1ppmにて検出される。化合物(D)、化合物(E)及び無機燐酸に由来する燐元素のピークは、いずれも+4~-1ppmにて検出されるが、低磁場側から、無機燐酸、化合物(E)、化合物(D)の順に帰属が決定される。
Compound (E) can be detected by the 31 P-NMR method in the same manner as compound (A).
The peak of phosphorus element derived from the compound (E) is detected at +4 to -1 ppm. The peak of phosphorus element derived from compound (D), compound (E) and inorganic phosphoric acid is detected at +4 to −1 ppm, but from the low magnetic field side, inorganic phosphoric acid, compound (E), compound (D ) Is determined in the order.
〔その他成分〕
 本発明の繊維処理剤は、上記で説明した化合物(A)、化合物(B)、化合物(D)、化合物(E)の他に、その他成分を含有してもよい。
 その他成分としては、本発明の効果を損なわない範囲で、たとえば、水;他の界面活性剤;消泡剤;防腐剤;脂肪酸アルキルエステル、パラフィンワックス、ジメチルシリコーン成分等の平滑剤等を挙げることができる。特に、合成繊維製造のための仕上工程で使用される場合、本発明の繊維処理剤が平滑剤をさらに含むことがある。
 他の界面活性剤としては、化合物(B)以外のノニオン界面活性剤等が挙げられる。
 化合物(B)以外のノニオン界面活性剤としては、ソルビタントリオレエート、グリセリンモノラウレート等の多価アルコール部分エステル型ノニオン界面活性剤、ポリオキシアルキレンソルビタントリオレエート、ポリオキシアルキレンヒマシ油、ポリオキシアルキレン硬化ヒマシ油トリオクタノエート等のポリオキシアルキレン多価アルコール脂肪酸エステル型ノニオン界面活性剤、エタノールアミンモノラウロアミド等のアルキルアミド型ノニオン界面活性剤、ポリオキシエチレンジエタノールアミンモノオレイルアミド等のポリオキシアルキレン脂肪酸アミド型ノニオン界面活性剤等が挙げられる
 本発明の繊維処理剤が水をさらに含む水性液(エマルション)になっていると、外観安定性および流動性という点で好ましい。
[Other ingredients]
The fiber treatment agent of the present invention may contain other components in addition to the compound (A), the compound (B), the compound (D), and the compound (E) described above.
Other components include, for example, water; other surfactants; antifoaming agents; preservatives; fatty acid alkyl esters, paraffin wax, smoothing agents such as dimethylsilicone components, etc., as long as the effects of the present invention are not impaired. Can do. In particular, when used in a finishing process for producing synthetic fibers, the fiber treatment agent of the present invention may further contain a smoothing agent.
Examples of other surfactants include nonionic surfactants other than the compound (B).
Nonionic surfactants other than compound (B) include polyhydric alcohol partial ester type nonionic surfactants such as sorbitan trioleate and glycerol monolaurate, polyoxyalkylene sorbitan trioleate, polyoxyalkylene castor oil, polyoxyalkylene Polyoxyalkylene polyhydric alcohol fatty acid ester type nonionic surfactant such as hydrogenated castor oil trioctanoate, alkylamide type nonionic surfactant such as ethanolamine monolauramide, and polyoxyalkylene such as polyoxyethylenediethanolamine monooleylamide Examples include fatty acid amide type nonionic surfactants. The fiber treatment agent of the present invention is preferably an aqueous liquid (emulsion) further containing water in terms of appearance stability and fluidity.
 本発明の繊維処理剤が水性液の場合、化合物(A)、化合物(B)、化合物(D)及び化合物(E)の合計量が繊維処理剤全体に占める配合割合については、特に限定はないが、好ましくは0.01~20重量%、より好ましくは0.02~10重量%、さらに好ましくは0.1~5重量%である。 When the fiber treatment agent of the present invention is an aqueous liquid, the blending ratio of the total amount of the compound (A), the compound (B), the compound (D) and the compound (E) in the entire fiber treatment agent is not particularly limited. However, it is preferably 0.01 to 20% by weight, more preferably 0.02 to 10% by weight, and still more preferably 0.1 to 5% by weight.
 化合物(A)、化合物(B)、化合物(D)及び化合物(E)の合計量が繊維処理剤全体に占める配合割合が、0.01重量%未満であると、所望の性能が得られない場合があり、繊維処理剤の給油工程において高めの含液率(給油される繊維処理剤重量の繊維重量に対する比率)が必要となるため、液垂れが多くなることがある。一方、20重量%超であると、繊維処理剤の安定性が悪くなり、化合物(A)の沈殿が発生し易くなり、溶液が増粘したりすることがある。 When the blending ratio of the total amount of the compound (A), the compound (B), the compound (D) and the compound (E) in the entire fiber treatment agent is less than 0.01% by weight, desired performance cannot be obtained. In some cases, since a higher liquid content (ratio of the weight of the fiber treatment agent to be fed to the fiber weight) is required in the fiber treatment agent refueling step, dripping may increase. On the other hand, if it exceeds 20% by weight, the stability of the fiber treatment agent becomes poor, precipitation of the compound (A) is likely to occur, and the solution may be thickened.
〔短繊維用繊維処理剤〕
 本発明の短繊維用繊維処理剤は、処理剤が付与されていない原料短繊維に対して付与するための繊維処理剤である。
 前記原料短繊維の繊維長は、9~64mmが好ましく、13~51mmがより好ましく、20~44mmがさらに好ましく、31~38mmが特に好ましい。繊維長が9mm未満及び64mm超であると、高速練条コイリング性が低下する可能性がある。
 前記原料短繊維の太さは、一般にデシテックス(以後、dtexで表現する)という単位で表されるが、0.7~4.0dtexが好ましく、0.8~3.0dtexがより好ましく、0.9~2.0dtexがさらに好ましく、1.0~1.5dtexが特に好ましい。0.7dtex未満では、カード通過性が低下するために、高速練条コイリング性が低下する可能性がある。4.0dtex超では、集束性が低下するために、高速練条コイリング性が低下する可能性がある。
[Fiber treatment agent for short fibers]
The fiber treatment agent for short fibers of the present invention is a fiber treatment agent for imparting to raw material short fibers to which no treatment agent is imparted.
The fiber length of the raw material short fibers is preferably 9 to 64 mm, more preferably 13 to 51 mm, still more preferably 20 to 44 mm, and particularly preferably 31 to 38 mm. If the fiber length is less than 9 mm and more than 64 mm, the high-speed drawing coiling property may be lowered.
The thickness of the raw short fiber is generally expressed in units of decitex (hereinafter expressed as dtex), preferably 0.7 to 4.0 dtex, more preferably 0.8 to 3.0 dtex, and 0.0. 9 to 2.0 dtex is more preferable, and 1.0 to 1.5 dtex is particularly preferable. If it is less than 0.7 dtex, the card passing property is lowered, so that the high-speed drawing coiling property may be lowered. If it exceeds 4.0 dtex, the focusing property is lowered, so that the high-speed drawing coiling property may be lowered.
 本発明の短繊維用繊維処理剤は、処理剤の不揮発分全体に占める前記化合物(A)の重量割合が1~16重量%であり、3~15重量%が好ましく、5~14重量%がより好ましく、7~13重量%がさらに好ましく、9~12重量%が最も好ましい。1重量%未満では化合物(A)の効果が発揮されず、練条コイリング性が低下する。16重量%超では、コイラープレートと繊維との摩擦が高くなるために、練条コイリング性が低下する。
 なお、本発明における不揮発分とは、処理剤を105℃で熱処理して溶媒等を除去し、恒量に達した時の絶乾成分をいう。
In the fiber treatment agent for short fibers of the present invention, the weight ratio of the compound (A) to the whole nonvolatile content of the treatment agent is 1 to 16% by weight, preferably 3 to 15% by weight, and preferably 5 to 14% by weight. More preferably, it is 7 to 13% by weight, further preferably 9 to 12% by weight. If it is less than 1% by weight, the effect of the compound (A) is not exhibited, and the strip coiling property is lowered. If it exceeds 16% by weight, the friction between the coiler plate and the fiber becomes high, so that the coiling property of the drawing is lowered.
The non-volatile content in the present invention refers to an absolutely dry component when the treatment agent is heat treated at 105 ° C. to remove the solvent and the like and reach a constant weight.
 前記化合物(A)及び前記化合物(B)の重量比率(A/B)は0.01~0.7であり、0.01~0.6が好ましく、0.03~0.6がより好ましく、0.07~0.6がさらに好ましく、0.1~0.5が特に好ましく、0.2~0.4が最も好ましい。0.01未満では、化合物(A)の重量が少ないために、練条コイリング性向上の効果は得られない。0.7超では、化合物(B)による、化合物(A)の乳化が不十分となり、練条コイリング性の効果は得られない。 The weight ratio (A / B) of the compound (A) and the compound (B) is 0.01 to 0.7, preferably 0.01 to 0.6, more preferably 0.03 to 0.6. 0.07 to 0.6 is more preferable, 0.1 to 0.5 is particularly preferable, and 0.2 to 0.4 is most preferable. If it is less than 0.01, since the weight of the compound (A) is small, the effect of improving the strip coiling property cannot be obtained. If it exceeds 0.7, emulsification of the compound (A) by the compound (B) becomes insufficient, and the effect of strip coiling property cannot be obtained.
 本発明の短繊維用繊維処理剤は、処理剤の不揮発分全体に占める無機燐酸の重量割合が1重量%以下であり、0.8重量%以下が好ましく、0.5重量%以下がさらに好ましく、0.3重量%未満が特に好ましい。好ましい下限値は0重量%である。無機燐酸が1重量%超であると、ゴム及び金属との親和性が強いため、練条工程において、練条コイラープレートに付着及び蓄積し、繊維―金属間の摩擦が急激に高くなることでコイリング性が低下する。 In the fiber treatment agent for short fibers of the present invention, the weight ratio of inorganic phosphoric acid to the entire nonvolatile content of the treatment agent is 1% by weight or less, preferably 0.8% by weight or less, and more preferably 0.5% by weight or less. , Less than 0.3% by weight is particularly preferred. A preferred lower limit is 0% by weight. If the inorganic phosphoric acid content exceeds 1% by weight, the affinity with rubber and metal is strong, so that in the drawing process, it adheres to and accumulates on the drawing coiler plate, and the friction between fiber and metal increases rapidly. Coiling performance decreases.
 無機燐酸は、化合物(A)と同様に、31P-NMRの方法で検出することができる。
 無機燐酸に由来する燐元素のピークは、+4~-1ppmにて検出される。化合物(D)、化合物(E)及び無機燐酸に由来する燐元素のピークは、いずれも+4~-1ppmにて検出されるが、低磁場側から、無機燐酸、化合物(E)、化合物(D)の順に帰属が決定される。
Inorganic phosphoric acid can be detected by the 31 P-NMR method as in the case of the compound (A).
The peak of phosphorus element derived from inorganic phosphoric acid is detected at +4 to -1 ppm. The peak of phosphorus element derived from compound (D), compound (E) and inorganic phosphoric acid is detected at +4 to −1 ppm, but from the low magnetic field side, inorganic phosphoric acid, compound (E), compound (D ) Is determined in the order.
 本発明の短繊維用繊維処理剤は、前記処理剤の不揮発分の吸湿率が1~15重量%であると好ましく、2~13重量%であるとより好ましく、3~11重量%であるとさらに好ましく、4~9重量%であると特に好ましい。この順に、紡績用処理剤の繊維-繊維間摩擦が適度となるために、練条コイリング性に優れる。吸湿率が1重量%未満では、繊維-繊維間摩擦が低すぎて、本願の効果が発揮されない可能性がある。15重量%を超えると繊維-繊維間摩擦が高すぎて、本願の効果が発揮されない可能性がある。
 ここでいう、処理剤の不揮発分の吸湿率は、次のようにして測定する。
(ア)絶乾した直径6cmのガラスシャーレを用意し、重量を測定する(W1)
(イ)前記シャーレに不揮発分が5重量%の繊維処理剤の水性液を20g入れ、3日間風乾した後、105℃、2時間で絶乾し、絶乾した処理剤を得る。この重量(絶乾した処理剤+ガラスシャーレ)を測定する(W2)。
(ウ)前記絶乾した処理剤を20℃、65%RHの環境で3日間放置し、吸湿した処理剤を得る。この重量(吸湿した処理剤+ガラスシャーレ)を測定する(W3)。
 吸湿率は次の式(1)の通りに計算する。
 吸湿率(重量%)=(W3-W2)/(W2-W1)×100   (1)
In the fiber treatment agent for short fibers of the present invention, the moisture absorption rate of the nonvolatile component of the treatment agent is preferably 1 to 15% by weight, more preferably 2 to 13% by weight, and more preferably 3 to 11% by weight. Further preferred is 4 to 9% by weight. In this order, the fiber-to-fiber friction of the spinning treatment agent becomes appropriate, and thus the coiling coiling property is excellent. If the moisture absorption rate is less than 1% by weight, the fiber-to-fiber friction is too low and the effects of the present application may not be exhibited. If it exceeds 15% by weight, the fiber-fiber friction is so high that the effects of the present application may not be exhibited.
The moisture absorption rate of the non-volatile content of the treating agent here is measured as follows.
(A) Prepare an absolutely dry glass petri dish with a diameter of 6 cm and measure the weight (W1)
(Ii) 20 g of an aqueous solution of a fiber treatment agent having a nonvolatile content of 5% by weight is put in the petri dish, and then air-dried for 3 days, and then absolutely dried at 105 ° C. for 2 hours to obtain an absolutely-dried treatment agent. This weight (absolutely dried treatment agent + glass petri dish) is measured (W2).
(C) The completely dried treatment agent is allowed to stand for 3 days in an environment of 20 ° C. and 65% RH to obtain a moisture-absorbing treatment agent. This weight (moisture absorbing treatment agent + glass petri dish) is measured (W3).
The moisture absorption rate is calculated as the following formula (1).
Moisture absorption rate (% by weight) = (W3-W2) / (W2-W1) × 100 (1)
 本発明の短繊維用繊維処理剤中に一定量含有されることで、処理剤が繊維に対して適度な繊維-繊維間摩擦を付与することができる観点から、処理剤の不揮発分全体に占める化合物(D)の重量割合は、25~50重量%であり、25~45重量%が好ましく、30~45重量%がより好ましい。 The treatment agent occupies the entire nonvolatile content of the treatment agent from the viewpoint that the treatment agent can impart an appropriate fiber-fiber friction to the fiber by being contained in a certain amount in the fiber treatment agent for short fibers of the present invention. The weight ratio of the compound (D) is 25 to 50% by weight, preferably 25 to 45% by weight, and more preferably 30 to 45% by weight.
 本発明の短繊維用繊維処理剤中に一定量含有されることで、処理剤が繊維に対して適度な繊維-繊維間摩擦を付与することができる観点から、処理剤の不揮発分全体に占める化合物(E)の重量割合は、20~40重量%であり、25~40重量%が好ましく、25~35重量%がより好ましい。 The treatment agent occupies the entire nonvolatile content of the treatment agent from the viewpoint that the treatment agent can impart an appropriate fiber-fiber friction to the fiber by being contained in a certain amount in the fiber treatment agent for short fibers of the present invention. The weight ratio of the compound (E) is 20 to 40% by weight, preferably 25 to 40% by weight, and more preferably 25 to 35% by weight.
 化合物(A)、化合物(D)、化合物(E)及び無機燐酸の合計重量に占める各化合物の重量は、繊維-金属間の摩擦が適度な値となり、練条コイリング性好ましい観点から、次に示す通りとなる。
 化合物(A)の重量割合が、化合物(A)、化合物(D)、化合物(E)及び無機燐酸の合計重量に対して、1~25重量%が好ましく、2~25重量%がより好ましく、3~20重量%がさらに好ましく、4~15重量%が特に好ましく、5~13重量%が最も好ましい。
The weight of each compound in the total weight of the compound (A), the compound (D), the compound (E) and the inorganic phosphoric acid is such that the friction between the fiber and the metal becomes an appropriate value, and from the viewpoint of the preferred strip coiling property, As shown.
The weight ratio of the compound (A) is preferably 1 to 25% by weight, more preferably 2 to 25% by weight, based on the total weight of the compound (A), the compound (D), the compound (E) and the inorganic phosphoric acid. It is more preferably 3 to 20% by weight, particularly preferably 4 to 15% by weight, and most preferably 5 to 13% by weight.
 化合物(D)の重量割合が、化合物(A)、化合物(D)、化合物(E)及び無機燐酸の合計重量に対して、20~60重量%が好ましく、25~55重量%がより好ましく、25~50重量%がさらに好ましく、25~45重量%がさらに好ましい。
 化合物(E)の重量割合が、化合物(A)、化合物(D)、化合物(E)及び無機燐酸の合計重量に対して、10~50重量%が好ましく、15~45重量%がより好ましく、20~40重量%がさらに好ましい。
 無機燐酸の重量割合が、化合物(A)、化合物(D)、化合物(E)及び無機燐酸の合計重量に対して、1.0重量%以下が好ましく、0.5重量%がより好ましく、0.2重量%がさらに好ましく、0.1重量%以下が特に好ましい。
The weight ratio of the compound (D) is preferably 20 to 60% by weight, more preferably 25 to 55% by weight, based on the total weight of the compound (A), the compound (D), the compound (E) and the inorganic phosphoric acid. It is more preferably 25 to 50% by weight, and further preferably 25 to 45% by weight.
The weight ratio of the compound (E) is preferably 10 to 50% by weight, more preferably 15 to 45% by weight, based on the total weight of the compound (A), the compound (D), the compound (E) and the inorganic phosphoric acid. More preferably, it is 20 to 40% by weight.
The weight ratio of the inorganic phosphoric acid is preferably 1.0% by weight or less, more preferably 0.5% by weight, based on the total weight of the compound (A), the compound (D), the compound (E) and the inorganic phosphoric acid. More preferably, it is 2% by weight, particularly preferably 0.1% by weight or less.
 本発明の短繊維用繊維処理剤は、短繊維用合成繊維を製造するための紡糸工程、延伸工程および仕上工程から選ばれる少なくとも1つの工程で使用される。
 本発明の短繊維用繊維処理剤は、紡績用であると、本願効果が発揮され易いことから好ましい。
The fiber treatment agent for short fibers of the present invention is used in at least one step selected from a spinning step, a drawing step and a finishing step for producing a synthetic fiber for short fibers.
The fiber treatment agent for short fibers of the present invention is preferably used for spinning because the effect of the present invention is easily exhibited.
 本発明の短繊維用繊維処理剤は、練条コイリング性が低下する観点から、処理剤の不揮発分全体に占める炭素数6~8のアルキル燐酸エステルカリウム塩の重量割合が10重量%未満であると好ましく、3重量%以下がより好ましく、2重量%以下がさらに好ましく、1重量%以下が特に好ましい。好ましい下限値は0重量%である。 In the fiber treatment agent for short fibers of the present invention, the weight ratio of the alkyl phosphate potassium salt having 6 to 8 carbon atoms in the entire nonvolatile content of the treatment agent is less than 10% by weight from the viewpoint of reducing the coiling property of the drawing. 3 wt% or less is more preferable, 2 wt% or less is more preferable, and 1 wt% or less is particularly preferable. A preferred lower limit is 0% by weight.
〔短繊維用繊維処理剤の製造方法〕
 本発明の短繊維用繊維処理剤は、化合物(A)を特定の比率で含有することを特徴とするが、本発明の短繊維用繊維処理剤の製造方法としては、有機燐酸化合物製造時に化合物(A)の含有比率を調整し、その後、化合物(B)等を配合する方法が挙げられる。
 具体的には、有機燐酸化合物は、有機ヒドロキシル化合物と無水燐酸とを反応させて反応物を得る工程(I)を行う。その後、水を前記反応物に添加して加水分解する工程(II)を行うことで、有機燐酸化合物に含まれる化合物(A)の比率を調整することができる。
 前記反応物に添加する水の量は、前記有機ヒドロキシル化合物に対して、0.01~1モルが好ましく、0.03~0.8モルがより好ましく、0.05~0.5モルがさらに好ましく、0.07~0.3モルが更に好ましい。0.01モル未満及び1モル超では、化合物(A)の量の調節が困難となる場合がある。
[Method for producing fiber treatment agent for short fibers]
The fiber treatment agent for short fibers of the present invention is characterized by containing the compound (A) in a specific ratio, and the method for producing the fiber treatment agent for short fibers of the present invention includes a compound at the time of producing the organic phosphate compound. A method of adjusting the content ratio of (A) and then blending the compound (B) and the like can be mentioned.
Specifically, an organic phosphoric acid compound performs the process (I) which makes an organic hydroxyl compound and phosphoric anhydride react, and obtains a reaction material. Then, the ratio of the compound (A) contained in the organic phosphoric acid compound can be adjusted by performing the step (II) of adding water to the reaction product and hydrolyzing it.
The amount of water added to the reaction product is preferably 0.01 to 1 mol, more preferably 0.03 to 0.8 mol, and even more preferably 0.05 to 0.5 mol with respect to the organic hydroxyl compound. Preferably, 0.07 to 0.3 mol is more preferable. If it is less than 0.01 mol and more than 1 mol, it may be difficult to adjust the amount of the compound (A).
 本発明の短繊維用繊維処理剤は、化合物(A)、化合物(D)、化合物(E)を含む水性液と、化合物(B)およびその他成分とを予め混合して得られる混合液と、必要に応じてその他成分とを混合することによって製造される。 The fiber treatment agent for short fibers of the present invention comprises a liquid mixture obtained by previously mixing an aqueous liquid containing the compound (A), the compound (D), and the compound (E) with the compound (B) and other components, Manufactured by mixing with other components as required.
 本発明の短繊維用繊維処理剤を製造するための原料を取扱、保管、運搬等する場合、化合物(A)は、これ以外の成分(具体的には、化合物(B)及び必要に応じて使用するその他の使用成分から選ばれる少なくとも1種)と共存させない方が好ましい。化合物(A)にこれ以外の成分を共存させた場合、得られる本発明の繊維処理剤の製品安定性が悪くなり、経時により分離や凝集などの外観不良を起こすことがある。なお、化合物(D)及び化合物(E)を共存させても、得られる本発明の繊維処理剤の製品安定性は良好であり問題はない。 When the raw material for producing the fiber treatment agent for short fibers of the present invention is handled, stored, transported, etc., the compound (A) is composed of other components (specifically, the compound (B) and as necessary. It is preferable not to coexist with at least one selected from other used components to be used. When a component other than this is coexisted with the compound (A), the product stability of the resulting fiber treating agent of the present invention is deteriorated, and appearance defects such as separation and aggregation may occur over time. In addition, even if a compound (D) and a compound (E) coexist, the product stability of the fiber treatment agent of this invention obtained is favorable, and there is no problem.
〔短繊維〕
 本発明の短繊維は、原料短繊維に対して、本発明の短繊維用繊維処理剤が付与されたものである。
[Short fiber]
The short fiber of the present invention is obtained by adding the fiber treatment agent for short fiber of the present invention to the raw short fiber.
 短繊維用繊維処理剤の付与量は、原料短繊維に対して、0.05~2.0重量%であり、0.06~1.5重量%が好ましく、0.07~1.0重量%がさらに好ましく、0.08~0.7重量%が最も好ましい。0.05%未満及び2.0重量%超では、紡績工程のカード通過性が劣る可能性がある。 The application amount of the fiber treatment agent for short fibers is 0.05 to 2.0% by weight, preferably 0.06 to 1.5% by weight, and 0.07 to 1.0% by weight based on the raw short fibers. % Is more preferable, and 0.08 to 0.7% by weight is most preferable. If it is less than 0.05% and more than 2.0% by weight, the card passing property in the spinning process may be inferior.
 本発明の短繊維用繊維処理剤は、そのまま希釈等せずに原料短繊維本体に付着させてもよく、水等で不揮発分全体の重量割合が0.01~10重量%となる濃度に希釈してエマルジョンとして原料短繊維本体に付着させてもよい。短繊維用繊維処理剤を原料短繊維本体へ付着させる工程は、原料短繊維本体の紡糸工程、延伸工程、捲縮工程、切断工程手前等のいずれであってもよい。本発明の短繊維用繊維処理剤を原料短繊維本体に付着させる手段については、特に限定はなく、ローラー給油、ノズルスプレー給油、ディップ給油等の手段を使用してもよい。短繊維の製造工程やその特性に合わせ、より均一に効率よく目的の付着率が得られる方法を採用すればよい。また、乾燥の方法としては、熱風および赤外線により乾燥させる方法、熱源に接触させて乾燥させる方法等を用いてよい。 The fiber treatment agent for short fibers of the present invention may be adhered to the raw material short fiber main body without being diluted as it is, and diluted with water to a concentration such that the weight ratio of the entire nonvolatile content becomes 0.01 to 10% by weight. And you may make it adhere to the raw material short fiber main body as an emulsion. The step of adhering the fiber treatment agent for short fibers to the raw material short fiber body may be any of the spinning process, drawing process, crimping process, cutting process and the like of the raw material short fiber body. The means for attaching the fiber treatment agent for short fibers of the present invention to the raw short fiber body is not particularly limited, and means such as roller oil supply, nozzle spray oil supply, and dip oil supply may be used. A method for obtaining the desired adhesion rate more uniformly and efficiently may be adopted in accordance with the short fiber manufacturing process and its characteristics. Moreover, as a drying method, you may use the method of drying with a hot air and infrared rays, the method of making it contact with a heat source, and drying.
 本発明の原料短繊維としては、木綿繊維、晒し処理された木綿繊維等の天然繊維、レーヨン繊維、キュプラ繊維、アセテート繊維等の再生繊維、ポリオレフィン繊維、ポリエステル繊維、ポリアミド繊維、アクリル繊維、ポリ塩化ビニル繊維、2種類以上の熱可塑性樹脂からなる複合繊維等の合成繊維が挙げられる。ポリアミド繊維としては、6-ナイロン繊維、6,6-ナイロン繊維、芳香族ポリアミド繊維等が挙げられる。 The raw material short fibers of the present invention include cotton fibers, natural fibers such as bleached cotton fibers, regenerated fibers such as rayon fibers, cupra fibers, acetate fibers, polyolefin fibers, polyester fibers, polyamide fibers, acrylic fibers, polychlorinated fibers. Examples thereof include synthetic fibers such as vinyl fibers and composite fibers composed of two or more kinds of thermoplastic resins. Examples of the polyamide fiber include 6-nylon fiber, 6,6-nylon fiber, and aromatic polyamide fiber.
 レーヨン繊維としては、ビスコースレーヨン繊維、強力レーヨン繊維、高強力レーヨン繊維、高湿潤弾性レーヨン繊維、溶剤紡糸レーヨン繊維、ポリノジック繊維等が挙げられる。
 複合繊維の組み合わせとしては、ポリオレフィン系樹脂/ポリオレフィン系樹脂の場合、例えば、高密度ポリエチレン/ポリプロピレン、直鎖状高密度ポリエチレン/ポリプロピレン、低密度ポリエチレン/ポリプロピレン、プロピレンと他のα-オレフィンとの二元共重合体又は三元共重合体/ポリプロピレン、直鎖状高密度ポリエチレン/高密度ポリエチレン、低密度ポリエチレン/高密度ポリエチレン等が挙げられる。また、ポリオレフィン系樹脂/ポリエステル系樹脂の場合、例えば、ポリプロピレン/ポリエチレンテレフタレート、高密度ポリエチレン/ポリエチレンテレフタレート、直鎖状高密度ポリエチレン/ポリエチレンテレフタレート、低密度ポリエチレン/ポリエチレンテレフタレート等が挙げられる。また、ポリエステル系樹脂/ポリエステル系樹脂の場合、例えば、共重合ポリエステル/ポリエチレンテレフタレート等が挙げられる。さらにポリアミド系樹脂/ポリエステル系樹脂、ポリオレフィン系樹脂/ポリアミド系樹脂等からなる繊維も挙げられる。
 これらの中でも、原料繊維がポリエステル繊維であれば、つや消し剤として内添している酸化チタンの量が適切でない場合には、特に練条コイリング性が低下する傾向にあることから、原料繊維がポリエステル繊維であることが、好ましい。
 ポリエステル繊維中に含まれる前記酸化チタンの重量割合は、本願効果をより発揮し易い観点から、1500~4000ppmが好ましく、1700~3500ppmがより好ましく、2000~3000ppmがさらに好ましい。
Examples of the rayon fiber include viscose rayon fiber, strong rayon fiber, high strength rayon fiber, high wet elastic rayon fiber, solvent-spun rayon fiber, and polynosic fiber.
As the combination of the composite fibers, in the case of polyolefin resin / polyolefin resin, for example, high density polyethylene / polypropylene, linear high density polyethylene / polypropylene, low density polyethylene / polypropylene, two types of propylene and other α-olefins are used. Examples thereof include an original copolymer or a terpolymer / polypropylene, linear high-density polyethylene / high-density polyethylene, and low-density polyethylene / high-density polyethylene. In the case of polyolefin resin / polyester resin, for example, polypropylene / polyethylene terephthalate, high-density polyethylene / polyethylene terephthalate, linear high-density polyethylene / polyethylene terephthalate, and low-density polyethylene / polyethylene terephthalate. Moreover, in the case of polyester-type resin / polyester-type resin, copolymer polyester / polyethylene terephthalate etc. are mentioned, for example. Furthermore, the fiber which consists of polyamide-type resin / polyester-type resin, polyolefin-type resin / polyamide-type resin, etc. is mentioned.
Among these, if the raw material fiber is a polyester fiber, if the amount of titanium oxide internally added as a matting agent is not suitable, the raw material fiber tends to be deteriorated, particularly, the coiling property tends to be reduced. A fiber is preferable.
The weight ratio of the titanium oxide contained in the polyester fiber is preferably 1500 to 4000 ppm, more preferably 1700 to 3500 ppm, and still more preferably 2000 to 3000 ppm from the viewpoint that the effect of the present application is more easily exhibited.
 繊維の断面形状は円形又は異形形状とすることができる。異形形状の場合、例えば扁平型、三角形~八角形等の多角型、T字型、中空型、多葉型等の任意の形状とすることができる。また、繊維の断面構造は鞘芯型、並列型、偏心鞘芯型、多層型、放射型あるいは海島型が例示できるが、繊維製造工程での生産性の容易さから、偏心を含む鞘芯型又は並列型が好ましい。 The cross-sectional shape of the fiber can be circular or irregular. In the case of an irregular shape, for example, a flat shape, a polygonal shape such as a triangle to an octagon, a T shape, a hollow shape, a multileaf shape, and the like can be used. The cross-sectional structure of the fiber can be exemplified by a sheath core type, a parallel core type, an eccentric sheath core type, a multilayer type, a radiation type, or a sea island type. Or a parallel type is preferable.
 本発明の短繊維の繊維長は、9~64mmが好ましく、13~51mmがより好ましく、20~44mmがさらに好ましく、31~38mmが特に好ましい。繊維長が9mm未満及び64mm超であると、高速練条コイリング性が低下する可能性がある。
 本発明の短繊維の太さは、一般にデシテックス(以後、dtexで表現する)という単位で表されるが、0.7~4.0dtexが好ましく、0.8~3.0dtexがより好ましく、0.9~2.0dtexがさらに好ましく、1.0~1.5dtexが特に好ましい。0.7dtex未満では、カード通過性が低下するために、高速練条コイリング性が低下する可能性がある。4.0dtex超では、集束性が低下するために、高速練条コイリング性が低下する可能性がある。
 本発明の短繊維は、本願効果を発揮し易い観点から、紡績用であることが好ましい。
The fiber length of the short fiber of the present invention is preferably 9 to 64 mm, more preferably 13 to 51 mm, still more preferably 20 to 44 mm, and particularly preferably 31 to 38 mm. If the fiber length is less than 9 mm and more than 64 mm, the high-speed drawing coiling property may be lowered.
The thickness of the short fiber of the present invention is generally expressed in units of decitex (hereinafter expressed as dtex), preferably 0.7 to 4.0 dtex, more preferably 0.8 to 3.0 dtex, 0 Is more preferably 0.9 to 2.0 dtex, and particularly preferably 1.0 to 1.5 dtex. If it is less than 0.7 dtex, the card passing property is lowered, so that the high-speed drawing coiling property may be lowered. If it exceeds 4.0 dtex, the focusing property is lowered, so that the high-speed drawing coiling property may be lowered.
The short fiber of the present invention is preferably used for spinning from the viewpoint of easily exerting the effect of the present application.
 以下に本発明を実施例によって説明するが、本発明はこれに限定されるものではない。尚、各実施例、比較例における評価項目と評価方法は以下の通りである。又、各実施例、比較例における処理剤の明細と評価結果を表3にまとめて示す。処理剤の明細中、配合比率はいずれも重量%を表す。 Hereinafter, the present invention will be described by way of examples, but the present invention is not limited thereto. In addition, the evaluation items and the evaluation method in each example and comparative example are as follows. In addition, Table 3 summarizes the details and evaluation results of the treatment agents in each Example and Comparative Example. In the description of the treatment agent, the blending ratios all represent weight percent.
31P-NMR測定方法〕
 燐酸化合物中の化合物(A)、化合物(D)、化合物(E)及び無機燐酸の比率を、31P-NMR測定方法により測定した。
 測定試料不揮発分約30mgを直径5mmのNMR用試料管に秤量し、重水素化溶媒として約0.5mlの重水(DO)を加え溶解させて、31P-NMR測定装置(BRUKER社製AVANCE400,162MHz)で測定した。
 化合物(A)に由来する燐元素のピークは、-5~-15ppmにて検出される。
 化合物(D)、化合物(E)及び無機燐酸に由来する燐元素のピークは、いずれも+4~-1ppmにて検出されるが、低磁場側から、無機燐酸、化合物(E)、化合物(D)の順に帰属が決定される。
 帰属後、積分比率から化合物(A)、無機燐酸、化合物(E)及び化合物(D)の比率を計算した。
[31 P-NMR measurement method]
The ratio of compound (A), compound (D), compound (E) and inorganic phosphoric acid in the phosphoric acid compound was measured by a 31 P-NMR measurement method.
About 30 mg of the measurement sample non-volatile content was weighed into an NMR sample tube having a diameter of 5 mm, dissolved by adding about 0.5 ml of heavy water (D 2 O) as a deuterated solvent, and 31 P-NMR measurement apparatus (manufactured by BRUKER) (AVANCE 400, 162 MHz).
The peak of phosphorus element derived from the compound (A) is detected at -5 to -15 ppm.
The peak of phosphorus element derived from compound (D), compound (E) and inorganic phosphoric acid is detected at +4 to −1 ppm, but from the low magnetic field side, inorganic phosphoric acid, compound (E), compound (D ) Is determined in the order.
After the assignment, the ratio of compound (A), inorganic phosphoric acid, compound (E) and compound (D) was calculated from the integral ratio.
〔製造例1~8〕
 まず、化合物(A)、化合物(D)、化合物(E)及び無機燐酸の混合物である有機燐酸化合物を次のように製造した。
[Production Examples 1 to 8]
First, an organic phosphoric acid compound, which is a mixture of compound (A), compound (D), compound (E) and inorganic phosphoric acid, was produced as follows.
(製造例1)
 ステアリルアルコール250gを1リットルフラスコに仕込み、攪拌しながら徐々に無水燐酸52.6g(ステアリルアルコール1モルに対してPとして0.40モルに相当)を投入し、80℃を保持したまま、3時間攪拌した。その後、イオン交換水(1)1.7g(ステアリルアルコール1モルに対して0.1モルに相当)を投入し、80℃で30分~1時間攪拌した。微褐色透明未中和物が得られた。
 イオン交換水(2)441.7g及び50%重量濃度KOH溶液106.5gを別の1リットルフラスコに仕込み、攪拌しながら、前記未中和物を徐々に投入し、白色ペースト(不揮発分40%、水分60%)を得た。
 当該白色ペーストの組成を31P-NMRで確認すると、化合物(A)が、前記白色ペーストの不揮発分全体に対して3重量%、化合物(D)が、前記白色ペーストの不揮発分全体に対して54.9重量%、化合物(E)が、前記白色ペーストの不揮発分全体に対して42重量%、無機燐酸が、前記白色ペーストの不揮発分全体に対して0.1重量%であることが確認された。
(Production Example 1)
Stearyl alcohol 250 g was charged into a 1 liter flask, and while stirring, 52.6 g of phosphoric anhydride (corresponding to 0.40 mol as P 2 O 5 with respect to 1 mol of stearyl alcohol) was gradually added and kept at 80 ° C. Stir for 3 hours. Thereafter, 1.7 g of ion-exchanged water (1) (corresponding to 0.1 mol per 1 mol of stearyl alcohol) was added and stirred at 80 ° C. for 30 minutes to 1 hour. A slightly brown transparent unneutralized product was obtained.
Charge 441.7 g of ion-exchanged water (2) and 106.5 g of 50% weight-concentrated KOH solution into another 1 liter flask, gradually add the unneutralized product while stirring, and add white paste (non-volatile content 40% , Moisture 60%).
When the composition of the white paste was confirmed by 31 P-NMR, the compound (A) was 3% by weight with respect to the total nonvolatile content of the white paste, and the compound (D) was based on the total nonvolatile content of the white paste. It was confirmed that 54.9% by weight, compound (E) was 42% by weight with respect to the entire nonvolatile content of the white paste, and inorganic phosphoric acid was 0.1% by weight with respect to the entire nonvolatile content of the white paste. It was done.
(製造例2及び3)
 イオン交換水(1)の量を表1の量に変更する以外は製造例1と同様にして、製造例2及び製造例3の燐酸化合物を得た。得られた化合物(A)、化合物(D)、化合物(E)及び無機燐酸の比率は、表1に示す通りであった。
(Production Examples 2 and 3)
The phosphoric acid compounds of Production Example 2 and Production Example 3 were obtained in the same manner as in Production Example 1 except that the amount of ion-exchanged water (1) was changed to the amount shown in Table 1. The ratio of the obtained compound (A), compound (D), compound (E) and inorganic phosphoric acid was as shown in Table 1.
(製造例4~6)
 ステアリルアルコールをセチルアルコールに変更し、イオン交換水(1)の量を表1の量に変更する以外は製造例1と同様にして、製造例4~6の燐酸化合物を得た。得られた化合物(A)、化合物(D)、化合物(E)及び無機燐酸の比率は、表1に示す通りであった。
(Production Examples 4 to 6)
The phosphoric acid compounds of Production Examples 4 to 6 were obtained in the same manner as in Production Example 1 except that stearyl alcohol was changed to cetyl alcohol and the amount of ion-exchanged water (1) was changed to the amount shown in Table 1. The ratio of the obtained compound (A), compound (D), compound (E) and inorganic phosphoric acid was as shown in Table 1.
(製造例7)
 ステアリルアルコール(純度99%以上)250gを1リットルフラスコに仕込み、攪拌しながら徐々に無水燐酸65.7g(ステアリルアルコール1モルに対してPとして0.50モルに相当)を投入し、80℃を保持したまま、3時間攪拌した。その後、イオン交換水(1)4g(ステアリルアルコール1モルに対して0.25モルに相当)を投入し、80℃で30分~1時間攪拌した。微褐色透明未中和物が得られた。
 イオン交換水(2)457.4g及び50%重量濃度KOH溶液171gを別の1リットルフラスコに仕込み、攪拌しながら、前記未中和物を徐々に投入し、白色ペースト(不揮発分40%、水分60%)を得た。当該白色ペーストの組成を31P-NMRで確認すると、化合物(A)、化合物(D)、化合物(E)及び無機燐酸の比率は、表1に示す通りであった。
(製造例8)
 ステアリルアルコール(純度99%以上)250gを1リットルフラスコに仕込み、攪拌しながら徐々に無水燐酸59.3g(ステアリルアルコール1モルに対してPとして0.45モルに相当)を投入した。無色透明未中和物が得られた。
 イオン交換水(2)444.4g及び50%重量濃度KOH溶液129.6gを別の1リットルフラスコに仕込み、攪拌しながら、前記未中和物を徐々に投入し、白色ペースト(不揮発分40%、水分60%)を得た。当該白色ペーストの組成を31P-NMRで確認すると、化合物(A)、化合物(D)、化合物(E)及び無機燐酸の比率は、表1に示す通りであった。
(Production Example 7)
Stearyl alcohol (purity 99% or more) 250 g was charged into a 1 liter flask, and 65.7 g of phosphoric anhydride (corresponding to 0.50 mol as P 2 O 5 with respect to 1 mol of stearyl alcohol) was gradually added while stirring. The mixture was stirred for 3 hours while maintaining 80 ° C. Thereafter, 4 g of ion-exchanged water (1) (corresponding to 0.25 mol with respect to 1 mol of stearyl alcohol) was added and stirred at 80 ° C. for 30 minutes to 1 hour. A slightly brown transparent unneutralized product was obtained.
Charge 457.4 g of ion-exchanged water (2) and 171 g of 50% weight-concentrated KOH solution into another 1 liter flask, gradually add the unneutralized product while stirring, and add white paste (non-volatile content 40%, moisture content) 60%). When the composition of the white paste was confirmed by 31 P-NMR, the ratio of compound (A), compound (D), compound (E) and inorganic phosphoric acid was as shown in Table 1.
(Production Example 8)
Stearyl alcohol (purity 99% or more) 250 g was charged into a 1 liter flask, and 59.3 g of phosphoric anhydride (corresponding to 0.45 mol as P 2 O 5 with respect to 1 mol of stearyl alcohol) was gradually added while stirring. A colorless and transparent unneutralized product was obtained.
Charge 444.4 g of ion-exchanged water (2) and 129.6 g of 50% weight-concentrated KOH solution into another 1 liter flask, gradually add the unneutralized product while stirring, and add white paste (non-volatile content: 40% , Moisture 60%). When the composition of the white paste was confirmed by 31 P-NMR, the ratio of compound (A), compound (D), compound (E) and inorganic phosphoric acid was as shown in Table 1.
 表1に記載した上記製造例の燐酸化合物〔化合物(A)、化合物(D)、及び化合物(E)〕と、表2に記載した化合物(B1)と、次に示す化合物(B2)、化合物(F)、化合物(X)とを表3に記載の比率で混合を行い、撹拌して、各実施例・比較例の短繊維用繊維処理剤の不揮発分を調製した。前記不揮発分をイオン交換水で希釈して、0.5%濃度のエマルションを得た。 The phosphoric acid compounds [compound (A), compound (D), and compound (E)] of the above production example described in Table 1, the compound (B1) described in Table 2, the following compound (B2), and compound (F) and the compound (X) were mixed at the ratios shown in Table 3 and stirred to prepare nonvolatile components of the fiber treatment agents for short fibers of each Example and Comparative Example. The non-volatile component was diluted with ion-exchanged water to obtain a 0.5% concentration emulsion.
A-1 ポリステアリル燐酸エステルカリウム塩
A-2 ポリセチル燐酸エステルカリウム塩
B2-1 POE(10)アルキル(C12~13)アミノエーテル
B2-2 POE(7)アルキル(C12~13)アミノエーテル
B2-3 POE(12)アルキル(C12)アミノエーテル
D-1 ジステアリル燐酸エステルカリウム塩
D-2 ジセチル燐酸エステルカリウム塩
E-1 モノステアリル燐酸エステルカリウム塩
E-2 モノセチル燐酸エステルカリウム塩
F-1 パラフィンWAX乳化物(融点125°Fのもの。)
F-2 ジメチルシリコーン乳化物(粘度350cStのジメチルシリコーンを乳化したもの。)
X-1 ポリヘキシル燐酸エステルカリウム塩
X-2 ジヘキシル燐酸エステルカリウム塩
X-3 モノヘキシル燐酸エステルカリウム塩
A-1 Polystearyl phosphate potassium salt A-2 Polycetyl phosphate potassium salt B2-1 POE (10) alkyl (C 12-13 ) amino ether B2-2 POE (7) alkyl (C 12-13 ) amino ether B2 -3 POE (12) alkyl (C 12 ) amino ether D-1 Distearyl phosphate potassium salt D-2 Dicetyl phosphate potassium salt E-1 Monostearyl phosphate potassium salt E-2 Monocetyl phosphate potassium salt F-1 Paraffin WAX emulsion (melting point 125 ° F.)
F-2 Dimethyl silicone emulsion (Emulsified dimethyl silicone with a viscosity of 350 cSt)
X-1 Polyhexyl phosphate potassium salt X-2 Dihexyl phosphate potassium salt X-3 Monohexyl phosphate potassium salt
Figure JPOXMLDOC01-appb-T000014
Figure JPOXMLDOC01-appb-T000014
Figure JPOXMLDOC01-appb-T000015
Figure JPOXMLDOC01-appb-T000015
Figure JPOXMLDOC01-appb-T000016
Figure JPOXMLDOC01-appb-T000016
 次に、予め脱脂しておき、処理剤が付着していない1.3dtex×38mmの原料ポリエステル短繊維(TiO 2000ppm含有)10kgを用い、原料短繊維に対する処理剤の不揮発分の付着量が0.15重量%になるように、前記処理剤のエマルションを給油し、当該原綿を80℃、2時間で乾燥した。得られた処理剤付与綿を下記の各評価に供した。 Next, 10 kg of raw material polyester short fibers (containing 2000 ppm of TiO 2 ) of 1.3 dtex × 38 mm that have been degreased in advance and the treatment agent is not attached is used, and the non-volatile content of the treatment agent to the raw material short fibers is 0 The emulsion of the treatment agent was fed so as to be 15% by weight, and the raw cotton was dried at 80 ° C. for 2 hours. The obtained treatment agent-added cotton was subjected to the following evaluations.
[高速練条コイリング性評価方法]
 オープナーにより処理剤付与綿を開繊し、カード機を用いてカーディングして、カードスライバーを得た。
 30℃×80%RHの雰囲気下、カードスライバーを練条機(原織機製作所)に供し、紡出速度=700m/分の条件で5回通過させた。得られた練条スライバーのコイリング性を目視で判定した。判定基準は、次の通りで、○以上を合格とした。
 ◎:外観が非常に良好
 ○:コイリングフォームに1~3箇所の乱れが見られる。
 ×:コイリングフォームに4箇所以上の乱れが見られる。
[High speed drawing coiling evaluation method]
The treatment-applied cotton was opened with an opener and carded with a card machine to obtain a card sliver.
Under an atmosphere of 30 ° C. × 80% RH, the card sliver was supplied to a drawing machine (Hara Weaving Machine Works) and passed 5 times under the condition of spinning speed = 700 m / min. The coiling property of the obtained strip sliver was visually determined. Judgment criteria are as follows.
A: Appearance is very good A: Disturbances in 1 to 3 places are observed in the coiling foam.
X: Disturbance of four or more places is seen in coiling foam.
[制電性評価方法]
 下記の図1の4のゴムローラーから3cm離れた走行スライバーより1cmのところで春日式電位差測定装置で走行スライバーの静電気量を測定する。
 また、以下の評価基準で○以上を合格とした。
◎:2.0(kv)未満(非常に良好)
○:2.0以上10.0(kv)未満(良好)
×:10(kv)超(不良)
[Antistatic evaluation method]
The static electricity amount of the traveling sliver is measured with a Kasuga-type potentiometer at a distance of 1 cm from the traveling sliver 3 cm away from the rubber roller 4 in FIG.
Moreover, the above evaluation criteria set ○ or more as acceptable.
A: Less than 2.0 (kv) (very good)
○: 2.0 or more and less than 10.0 (kv) (good)
×: Over 10 (kv) (defect)
 表3から分かるように、実施例1~13の短繊維用繊維処理剤は、処理剤の不揮発分全体に占める前記化合物(A)の重量割合が1~16重量%であり、処理剤の不揮発分全体に占める前記化合物(D)の重量割合が25~50重量%であり、処理剤の不揮発分全体に占める前記化合物(E)の重量割合が20~40重量%であり、前記化合物(A)及び前記化合物(B)の重量比率(A/B)が0.01~0.70であり、無機燐酸の量が1重量%以下であるため、高速練条コイリング性が良好であった。
 一方、比較例1~5では、燐酸化合物である化合物(D)及び化合物(E)を含むが化合物(A)を含まない場合(比較例1)、化合物(A)が処理剤の不揮発分全体に対して30重量%を超えている場合(比較例2)、無機燐酸の量が処理剤の不揮発分全体に対して1重量%を超えている場合(比較例3)、化合物(A)は含有しているが化合物(A)及び前化合物(B)の重量比率(A/B)が0.01~0.70の範囲にない場合(比較例4)、化合物(A)を含有せず、化合物(B)のみを含有する場合(比較例5)には、高速練条コイリング性が劣っていた。
As can be seen from Table 3, in the fiber treatment agents for short fibers of Examples 1 to 13, the weight ratio of the compound (A) in the entire nonvolatile content of the treatment agent is 1 to 16% by weight, The weight ratio of the compound (D) in the total amount is 25 to 50% by weight, the weight ratio of the compound (E) in the non-volatile content of the treatment agent is 20 to 40% by weight, and the compound (A ) And the compound (B) in a weight ratio (A / B) of 0.01 to 0.70 and the amount of inorganic phosphoric acid is 1% by weight or less, the high-speed kneading coiling property was good.
On the other hand, in Comparative Examples 1 to 5, when the compound (D) and the compound (E) which are phosphoric acid compounds are included but the compound (A) is not included (Comparative Example 1), the compound (A) is the whole non-volatile content of the treating agent. When the amount exceeds 30% by weight (Comparative Example 2), when the amount of inorganic phosphoric acid exceeds 1% by weight with respect to the entire nonvolatile content of the treating agent (Comparative Example 3), the compound (A) is If it is contained but the weight ratio (A / B) of the compound (A) and the previous compound (B) is not in the range of 0.01 to 0.70 (Comparative Example 4), the compound (A) is not contained. When only compound (B) was contained (Comparative Example 5), the high-speed kneading coiling property was inferior.
 1 カードケンス
 2 カードスライバー
 3 ガイド
 4 ニップローラー
 5 コイラープレート
 6 練条ケンス
 7 練条スライバー
 8 コイリングフォームに乱れのないスライバー
 9 コイリングフォームに乱れのあるスライバー
1 Card Kens 2 Card Sliver 3 Guide 4 Nip Roller 5 Coiler Plate 6 Kenjo Ken 7 Rib Sliver 8 Sliver without disturbing coiling foam 9 Sliver with disturbing coiling foam
 本発明の短繊維用処理剤は、短繊維に対して高速練条コイリング性を付与することができるため、本発明の短繊維用繊維処理剤を付与した短繊維は、世界で急速に普及している高速紡績機械で紡績されても糸質に優れた精紡糸に仕上がる。 Since the treatment agent for short fibers of the present invention can impart high-speed drawing coiling properties to short fibers, the short fibers to which the fiber treatment agent for short fibers of the present invention has been imparted rapidly worldwide. Even if it is spun by a high-speed spinning machine, it is finished into a fine spun yarn with excellent yarn quality.

Claims (7)

  1.  短繊維用繊維処理剤であって、
    下記一般式(1)で表される化合物(A)と、下記一般式(2)で表される化合物(B1)及び下記一般式(3)で表される化合物(B2)から選ばれる少なくとも1種である化合物(B)と、下記一般式(4)で表される化合物(D)と、下記一般式(5)で表される化合物(E)とを必須に含有し、
    処理剤の不揮発分全体に占める前記化合物(A)の重量割合が1~16重量%であり、
    処理剤の不揮発分全体に占める前記化合物(D)の重量割合が25~50重量%であり、
    処理剤の不揮発分全体に占める前記化合物(E)の重量割合が20~40重量%であり、
    前記化合物(A)及び前記化合物(B)の重量比率(A/B)が0.01~0.70であり、
    処理剤の不揮発分全体に占める無機燐酸の重量割合が1重量%以下である、
    繊維処理剤。
    Figure JPOXMLDOC01-appb-C000001
    (式中、Rは炭素数16~18の直鎖のアルキル基である。Qは水素原子、アルカリ金属塩又は炭素数16~18の直鎖のアルキル基である。Qは、それぞれ独立して、水素原子又はアルカリ金属塩である。)
    Figure JPOXMLDOC01-appb-C000002
    (式中、Rは炭素数8~18のアルキル基、アルケニル基、アリール基又はアシル基を示し、直鎖又は分枝鎖のいずれの構造から構成されていてもよい。POはオキシプロピレン基、EOはオキシエチレン基、AOは炭素数2又は3のオキシアルキレン基を示す。a、b及びcは、各々の平均付加モル数を示し、aは0~10、bは0~10、cは1~20である。[(PO)/(EO)]はaモルのPOとbモルのEOとがランダム付加してなるポリオキシアルキレン基である。)
    Figure JPOXMLDOC01-appb-C000003
    (式中、AOは炭素数2又は3のオキシアルキレン基であり、m及びnはオキシアルキレン基の平均付加モル数を示し、m+nは2~20の数である。Rは炭素数8~16のアルキル基、アルケニル基又はアリール基を示し、直鎖又は分枝鎖のいずれの構造から構成されていてもよい。)
    Figure JPOXMLDOC01-appb-C000004
    (式中、Rは炭素数16~18の直鎖のアルキル基である。Rは炭素数16~18の直鎖のアルキル基である。Mは水素原子又はアルカリ金属塩である。)
    Figure JPOXMLDOC01-appb-C000005
    (式中、Rは炭素数16~18の直鎖のアルキル基である。MおよびMは、それぞれ独立して、水素原子又はアルカリ金属塩である。)
    A fiber treatment agent for short fibers,
    At least 1 selected from the compound (A) represented by the following general formula (1), the compound (B1) represented by the following general formula (2), and the compound (B2) represented by the following general formula (3) Containing essentially the compound (B) as a seed, the compound (D) represented by the following general formula (4), and the compound (E) represented by the following general formula (5),
    The weight ratio of the compound (A) to the whole nonvolatile content of the treating agent is 1 to 16% by weight,
    The weight ratio of the compound (D) to the whole nonvolatile content of the treating agent is 25 to 50% by weight,
    The weight ratio of the compound (E) to the entire nonvolatile content of the treating agent is 20 to 40% by weight,
    The weight ratio (A / B) of the compound (A) and the compound (B) is 0.01 to 0.70,
    The weight ratio of inorganic phosphoric acid in the entire nonvolatile content of the treatment agent is 1% by weight or less,
    Fiber treatment agent.
    Figure JPOXMLDOC01-appb-C000001
    (In the formula, R 1 .Q 2 is a straight-chain alkyl group .Q 1 is hydrogen atom, an alkali metal salt or linear alkyl group having 16 to 18 carbon atoms having 16 to 18 carbon atoms, respectively Independently, a hydrogen atom or an alkali metal salt.)
    Figure JPOXMLDOC01-appb-C000002
    (In the formula, R 2 represents an alkyl group, alkenyl group, aryl group or acyl group having 8 to 18 carbon atoms, and may be composed of either a linear or branched structure. PO is an oxypropylene group. , EO represents an oxyethylene group, and A 1 O represents an oxyalkylene group having 2 or 3 carbon atoms, a, b and c represent the average number of moles added, a being 0 to 10, and b being 0 to 10 , C is 1 to 20. [(PO) a / (EO) b ] is a polyoxyalkylene group formed by randomly adding a mole of PO and b mole of EO.)
    Figure JPOXMLDOC01-appb-C000003
    (In the formula, A 2 O is an oxyalkylene group having 2 or 3 carbon atoms, m and n are the average number of added moles of the oxyalkylene group, and m + n is a number from 2 to 20. R 3 is the number of carbon atoms. (8 to 16 alkyl groups, alkenyl groups or aryl groups, each of which may be composed of a linear or branched structure)
    Figure JPOXMLDOC01-appb-C000004
    (In the formula, R 4 is a linear alkyl group having 16 to 18 carbon atoms. R 5 is a linear alkyl group having 16 to 18 carbon atoms. M 1 is a hydrogen atom or an alkali metal salt. )
    Figure JPOXMLDOC01-appb-C000005
    (Wherein R 6 is a linear alkyl group having 16 to 18 carbon atoms. M 2 and M 3 are each independently a hydrogen atom or an alkali metal salt.)
  2.  前記Rは炭素数8~18のアルキル基、アルケニル基又はアリール基である、請求項1に記載の繊維処理剤。 2. The fiber treatment agent according to claim 1, wherein R 2 is an alkyl group, alkenyl group or aryl group having 8 to 18 carbon atoms.
  3.  前記化合物(B)は前記化合物(B1)であり、前記AOはオキシエチレン基である、請求項1又は2に記載の繊維処理剤。 The fiber treatment agent according to claim 1, wherein the compound (B) is the compound (B1), and the A 1 O is an oxyethylene group.
  4.  前記処理剤の不揮発分の吸湿率が1~15重量%である、請求項1~3のいずれかに記載の繊維処理剤。 The fiber treatment agent according to any one of claims 1 to 3, wherein the moisture content of the non-volatile component of the treatment agent is 1 to 15% by weight.
  5.  前記aが1~10及び前記bが1~10である、請求項1~4のいずれかに記載の繊維処理剤。 The fiber treating agent according to any one of claims 1 to 4, wherein the a is 1 to 10 and the b is 1 to 10.
  6.  処理剤の不揮発分全体に占める炭素数6~8のアルキル燐酸エステルカリウム塩の重量割合が3重量%未満である、請求項1~5のいずれかに記載の繊維処理剤。 The fiber treatment agent according to any one of claims 1 to 5, wherein a weight ratio of the alkyl phosphate ester potassium salt having 6 to 8 carbon atoms to the entire nonvolatile content of the treatment agent is less than 3% by weight.
  7.  請求項1~6のいずれかに記載の繊維処理剤が繊維本体に付与されてなる、短繊維。 A short fiber obtained by applying the fiber treatment agent according to any one of claims 1 to 6 to a fiber main body.
PCT/JP2014/080844 2014-04-30 2014-11-21 Agent for treating short-staple fibers and use for said agent WO2015166603A1 (en)

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