Treatment agent for recycled cellulose fiber, multi-component first treatment agent for recycled cellulose fiber, multi-component second treatment agent for recycled cellulose fiber, and use thereof
A treatment agent with a specific organic phosphate ester compound and nonionic surfactant ratio addresses fiber opening issues in regenerated cellulose fibers, enhancing nep suppression and quality in spun yarn and nonwoven fabrics.
Patent Information
- Application Number
- PCT/JP2025/016254
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-05-10
- Filing Date
- 2025-04-28
- Publication Date
- 2025-11-13
AI Technical Summary
Conventional treatment agents for regenerated cellulose fibers result in defects such as knotting and nep formation during spun yarn and nonwoven fabric production due to insufficient fiber opening, leading to poor quality.
A treatment agent for regenerated cellulose fibers comprising a specific organic phosphate ester compound and a nonionic surfactant in a defined weight ratio, enhancing fiber openability and nep suppression.
The treatment agent improves fiber uniformity and quality by effectively suppressing neps, resulting in high-quality spun yarn and nonwoven fabrics.
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Figure JP2025016254_13112025_PF_FP_ABST
Abstract
Description
Treatment agent for regenerated cellulose fibers, multi-component first treatment agent for regenerated cellulose fibers, multi-component second treatment agent for regenerated cellulose fibers, and use thereof
[0001] The present invention relates to a treatment agent for regenerated cellulose fibers and its use.
[0002] Regenerated cellulose fibers have attracted attention from the perspectives of global environmental conservation and sustainability due to their excellent biodegradability and the fact that they are made from plant-derived resources such as pulp and cotton linters. To improve processability in spinning and nonwoven fabric processing, regenerated cellulose fibers are sometimes treated with a treatment agent for regenerated cellulose fibers. Conventional treatment agents for regenerated cellulose fibers include those containing triglyceride sulfate as the main component (Patent Document 1) and those containing polyhydric alcohols, fatty acids, and nonionic surfactants as the main components (Patent Document 2).
[0003] Japanese Patent Publication No. 2015-206128 Japanese Patent Publication No. 2020-2497
[0004] However, with these conventional treatment agents, in the spun yarn production process and nonwoven fabric production process, which have recently been required to be faster, there has been a problem that defects such as knotting and neps occur due to insufficient fiber opening, and sufficient uniformity cannot be obtained, resulting in a decrease in the quality of the spun yarn and nonwoven fabric. Therefore, an object of the present invention is to provide a treatment agent for regenerated cellulose fibers that is excellent in nep suppression, a multi-component first treatment agent for regenerated cellulose fibers that can be used as the treatment agent, a multi-component second treatment agent for regenerated cellulose fibers that can be used as the treatment agent, regenerated cellulose fibers to which the treatment agent has been attached, and spun yarn containing the fibers.
[0005] As a result of intensive research to solve the above-mentioned problems, the present inventors have discovered that the problem can be solved by using a treatment agent for regenerated cellulose fibers containing a specific organic phosphate ester compound (A) and a nonionic surfactant (B) in a specific weight ratio.
[0006] That is, the water permeability imparting agent of the present invention includes the following embodiments. <1> A treating agent for regenerated cellulose fibers, comprising the following organic phosphate ester compound (A) and nonionic surfactant (B), wherein the weight ratio (A / B) of the compound (A) to the surfactant (B) is 0.05 to 1.0. Organic phosphate ester compound (A): An organic phosphate ester compound having a hydrocarbon group having 14 to 22 carbon atoms, including a compound (A1) represented by the following general formula (1) and a compound (A2) represented by the following general formula (2): (In formula (1), R 1 is a monovalent saturated hydrocarbon group having 14 to 22 carbon atoms. 1 and M 2 are each independently a hydrogen atom, an alkali metal, ammonium, phosphonium, an organic amine, or a quaternary ammonium. (In formula (2), R 2 and R 3 are each independently a monovalent saturated hydrocarbon group having 14 to 22 carbon atoms. 1 is a hydrogen atom, an alkali metal, ammonium, phosphonium, an organic amine, or a quaternary ammonium.) <2> The treatment agent for regenerated cellulose fibers according to <1>, wherein the compound (A) optionally contains a compound (A3) represented by the following general formula (3), and the weight ratio of the compound (A1) to the total of the compounds (A1), (A2), and (A3) (A1 / (A1+A2+A3)) is 0.01 to 0.6: (In formula (3), R 4 is a monovalent saturated hydrocarbon group having 14 to 22 carbon atoms. 1 and M 2 are each independently a hydrogen atom, an alkali metal, ammonium, phosphonium, an organic amine, or a quaternary ammonium. 2 or R 5 It is. 5 is a monovalent saturated hydrocarbon group having 14 to 22 carbon atoms. Y is 1 or 2. M 2When there are two or more R , they may be the same or different.) <3> The treatment agent for regenerated cellulose fibers according to <2>, wherein the compound (A) contains a compound (A3) represented by the general formula (3). <4> The treatment agent for regenerated cellulose fibers according to <2>, wherein the compound (A) contains a compound (A3) represented by the general formula (3). 1 is a monovalent saturated hydrocarbon group having 16 to 22 carbon atoms; and 2 and R 3 wherein each independently represents a monovalent saturated hydrocarbon group having 16 to 22 carbon atoms. <5> The treatment agent for regenerated cellulose fibers according to any one of <1> to <4>, wherein the acid value of the nonvolatile content of the treatment agent for regenerated cellulose fibers is 0.1 to 70 mg KOH / g. <6> The treatment agent for regenerated cellulose fibers according to any one of <1> to <5>, wherein the nonionic surfactant (B) comprises at least one selected from the group consisting of a compound represented by the following general formula (4) and a nitrogen-containing nonionic surfactant: (In formula (4), R 6 is an alkyl group having 8 to 22 carbon atoms, an alkenyl group having 8 to 22 carbon atoms, an alkanoyl group having 8 to 22 carbon atoms, or an alkenoyl group having 8 to 22 carbon atoms. 7 is a hydrogen atom, an alkyl group having 8 to 22 carbon atoms, an alkenyl group having 8 to 22 carbon atoms, an alkanoyl group having 8 to 22 carbon atoms, or an alkenoyl group having 8 to 22 carbon atoms. a and b are each an integer of 0 to 20, and satisfy the relationship 3≦a+b≦40. 3 H 6 O) and (C 2 H 4and O) may be arranged randomly or may form blocks.) <7> The treatment agent for regenerated cellulose fibers according to any one of <1> to <6>, which is used for spinning regenerated cellulose. <8> The treatment agent for regenerated cellulose fibers according to any one of <1> to <7>, which is composed of a plurality of treatment agent sets including a multi-component first treatment agent for regenerated cellulose fibers containing the compound (A) and a multi-component second treatment agent for regenerated cellulose fibers containing the nonionic surfactant (B). <9> A multi-component first treatment agent for regenerated cellulose fibers used as the treatment agent for regenerated cellulose fibers according to any one of <1> to <7>, wherein the treatment agent for regenerated cellulose fibers is composed of a plurality of treatment agent sets, and the multi-component first treatment agent for regenerated cellulose fibers containing the compound (A) is used in combination with a multi-component second treatment agent for regenerated cellulose fibers containing the nonionic surfactant (B). <10> A multi-component second treatment agent for regenerated cellulose fibers, used as the treatment agent for regenerated cellulose fibers according to any one of <1> to <7>, wherein the treatment agent for regenerated cellulose fibers is a treatment agent for regenerated cellulose fibers composed of a plurality of treatment agent sets, and the multi-component second treatment agent for regenerated cellulose fibers contains the nonionic surfactant (B), and is used in combination with a multi-component first treatment agent for regenerated cellulose fibers containing the compound (A). <11> Regenerated cellulose fibers to which the treatment agent for regenerated cellulose fibers according to any one of <1> to <8> has been applied. <12> Spun yarn, comprising the regenerated cellulose fibers according to <11>.
[0007] The regenerated cellulose fiber treating agent of the present invention has excellent nep-suppressing properties. Because the regenerated cellulose fiber of the present invention is treated with a fiber treating agent having excellent nep-suppressing properties, regenerated cellulose fiber having excellent nep-suppressing properties and excellent quality can be obtained. Because the spun yarn of the present invention contains regenerated cellulose fiber to which a fiber treating agent having excellent nep-suppressing properties has been treated, spun yarn of excellent quality can be obtained.
[0008] Schematic diagram showing the definition of U%
[0009] The treating agent for regenerated cellulose fibers of the present invention (hereinafter sometimes simply referred to as the treating agent) contains an organic phosphate ester compound (A) and a nonionic surfactant (B) described below in specific proportions.
[0010] [Organophosphate Ester Compound (A)] The organic phosphate ester compound (A) (hereinafter, sometimes simply referred to as compound (A)) is an organic phosphate ester compound having a hydrocarbon group having 14 to 22 carbon atoms, including the compound (A1) represented by the general formula (1) above and the compound (A2) represented by the general formula (2) above.
[0011] [Compound (A1) represented by general formula (1)] The organic phosphate ester compound (A) includes the compound (A1) represented by the above general formula (1) (hereinafter, sometimes simply referred to as compound (A1)). The compound (A1) is not particularly limited as long as it is a compound represented by general formula (1), and one or more types may be used in combination. In general formula (1), R 1 is a monovalent saturated hydrocarbon group having 14 to 22 carbon atoms. From the viewpoint of excellent fiber openability in the spun yarn production process and the nonwoven fabric production process, the upper limit of the number of carbon atoms is preferably 20, more preferably 18, and the lower limit of the number of carbon atoms is preferably 15, more preferably 16. Furthermore, for example, 16 to 22 is preferred, and 16 to 18 is more preferred.
[0012] R 1 There are no particular limitations on the group, but examples thereof include an n-tetradecyl group, an n-pentadecyl group, an n-hexadecyl group, an n-heptadecyl group, an n-octadecyl group, an n-icosyl group, an n-docosyl group, an iso-tetradecyl group, an iso-pentadecyl group, an iso-hexadecyl group, an iso-octadecyl group, a 2-hexyldecyl group, and a 2-octyldodecyl group.
[0013] In formula (1), M 1 and M 2 are each independently a hydrogen atom, an alkali metal, ammonium, phosphonium, an organic amine, or a quaternary ammonium. 1 and M 2 In terms of emulsion stability and antistatic properties, M is preferably a hydrogen atom, an alkali metal, or an organic amine.1 and M 2 may be the same or different. Examples of alkali metals include potassium, sodium, and lithium, with potassium or sodium being preferred in terms of emulsion stability and antistatic properties. Examples of organic amines include alkanolamines such as ethanolamine, diethanolamine, and triethanolamine, as well as triethylamine. Examples of quaternary ammoniums include alkyltrimethylammonium and dialkyldimethylammonium.
[0014] Specific examples of the compound (A1) include, but are not limited to, monotetradecyl phosphate disodium salt, monotetradecyl phosphate dipotassium salt, monohexadecyl phosphate, monohexadecyl phosphate monopotassium salt, monohexadecyl phosphate dipotassium salt, monohexadecyl phosphate bis(triethanolamine) salt, monooctadecyl phosphate, monooctadecyl phosphate monopotassium salt, monooctadecyl phosphate dipotassium salt, monooctadecyl phosphate bis(triethanolamine) salt, Examples include tadecyl phosphate bis(triethanolamine) salt, monoicosyl phosphate, monoicosyl phosphate monopotassium salt, monoicosyl phosphate dipotassium salt, monodocosyl phosphate, monodocosyl phosphate dipotassium salt, mono-iso-hexadecyl phosphate dipotassium salt, mono-iso-octadecyl phosphate dipotassium salt, mono-2-hexyldecyl phosphate dipotassium salt, mono-2-octyldodecyl phosphate dipotassium salt, etc. Among these, in terms of emulsion stability and fiber-opening ability, monohexadecyl phosphate monopotassium salt, monohexadecyl phosphate dipotassium salt, monooctadecyl phosphate monopotassium salt, monooctadecyl phosphate dipotassium salt, monoicosyl phosphate dipotassium salt, and monoiso-octadecyl phosphate dipotassium salt are preferred.
[0015] [Compound (A2) represented by general formula (2)] The organic phosphate ester compound (A) includes a compound (A2) represented by the general formula (2) (hereinafter, sometimes simply referred to as compound (A2)). The compound (A2) is not particularly limited as long as it is a compound represented by the general formula (2), and one or more types may be used in combination. In formula (2), R 2 and R 3 are each independently a monovalent saturated hydrocarbon group having 14 to 22 carbon atoms. From the viewpoint of excellent fiber openability in the spun yarn production process and the nonwoven fabric production process, the upper limit of the number of carbon atoms is preferably 20, more preferably 18, and the lower limit of the number of carbon atoms is preferably 15, more preferably 16. Furthermore, for example, 16 to 22 is preferred, and 16 to 18 is more preferred.
[0016] R 2 and R 3 There are no particular limitations on R, and examples thereof include an n-tetradecyl group, an n-pentadecyl group, a hexadecyl group, an n-heptadecyl group, an n-octadecyl group, an n-icosyl group, an n-docosyl group, an iso-tetradecyl group, an iso-pentadecyl group, an iso-hexadecyl group, an iso-octadecyl group, a hexyldecyl group, and an octyldodecyl group. 2 and R 3 may be the same or different.
[0017] In formula (2), M 1 is a hydrogen atom, an alkali metal, ammonium, phosphonium, an organic amine, or a quaternary ammonium. 1 In terms of emulsion stability and antistatic properties, the alkali metal is preferably an alkali metal or an organic amine. Examples of alkali metals include potassium, sodium, and lithium, and in terms of emulsion stability and antistatic properties, potassium or sodium is preferred. Examples of organic amines include alkanolamines such as ethanolamine, diethanolamine, and triethanolamine, and triethylamine. Examples of quaternary ammonium include alkyltrimethylammonium and dialkyldimethylammonium.
[0018] Specific examples of compound (A2) include, but are not limited to, ditetradecyl phosphate sodium salt, ditetradecyl phosphate potassium salt, dihexadecyl phosphate potassium salt, dihexadecyl phosphate triethanolamine salt, dioctadecyl phosphate potassium salt, dioctadecyl phosphate bis(triethanolamine) salt, diicosyl phosphate potassium salt, didocosyl phosphate potassium salt, di-iso-hexadecyl phosphate potassium salt, di-iso-octadecyl phosphate potassium salt, di-2-hexyldecyl phosphate potassium salt, di-2-octyldodecyl phosphate potassium salt, etc. Among these, dihexadecyl phosphate potassium salt, dioctadecyl phosphate potassium salt, diicosyl phosphate potassium salt, and di-iso-octadecyl phosphate potassium salt are preferred in terms of emulsion stability and fiber-opening ability.
[0019] [Compound (A3) represented by general formula (3)] The organic phosphate ester compound (A) may contain a compound (A3) represented by the above general formula (3) (hereinafter, sometimes simply referred to as compound (A3)). In terms of the stability of the treatment agent, it is preferable that the compound (A3) is contained. There are no particular limitations on the compound (A3) as long as it is a compound represented by the above general formula (3), and one or more types may be used in combination. In formula (3), R 4 and R 5 are each independently a monovalent saturated hydrocarbon group having 14 to 22 carbon atoms. From the viewpoint of excellent fiber openability in the spun yarn production process and nonwoven fabric production process, the upper limit of the carbon number is preferably 20, more preferably 18, and the lower limit of the carbon number is preferably 15, more preferably 16. Furthermore, for example, 16 to 22 is preferred, and 16 to 18 is more preferred. R 4 and R 5 There are no particular limitations on R, and examples thereof include an n-tetradecyl group, an n-pentadecyl group, an n-hexadecyl group, an n-heptadecyl group, an n-octadecyl group, an n-icosyl group, an n-docosyl group, an iso-tetradecyl group, an iso-pentadecyl group, an iso-hexadecyl group, an iso-octadecyl group, a 2-hexyldecyl group, and a 2-octyldodecyl group. 4 and R5 may be the same or different.
[0020] In formula (3), M 1 and M 2 are each independently a hydrogen atom, an alkali metal, ammonium, phosphonium, an organic amine, or a quaternary ammonium. 1 and M 2 In terms of emulsion stability and antistatic properties, M is preferably a hydrogen atom, an alkali metal, or an organic amine. 1 and M 2 may be the same or different. Examples of alkali metals include potassium, sodium, and lithium, with potassium or sodium being preferred in terms of emulsion stability and antistatic properties. Examples of organic amines include alkanolamines such as ethanolamine, diethanolamine, and triethanolamine, as well as triethylamine. Examples of quaternary ammoniums include alkyltrimethylammonium and dialkyldimethylammonium.
[0021] Q is M 2 or R 5 Y is 1 or 2. 2 When there are two or more, they may be the same or different.
[0022] Specific examples of the compound (A3) include, but are not limited to, monotetradecyl pyrophosphate disodium salt, monotetradecyl pyrophosphate trisodium salt, monotetradecyl pyrophosphate monopotassium salt, monotetradecyl pyrophosphate dipotassium salt, monotetradecyl pyrophosphate tripotassium salt, ditetradecyl pyrophosphate monopotassium salt, ditetradecyl pyrophosphate dipotassium salt, monohexadecyl pyrophosphate monopotassium salt, monohexadecyl pyrophosphate dipotassium salt, monohexadecyl pyrophosphate Phosphate tripotassium salt, dihexadecyl pyrophosphate monopotassium salt, dihexadecyl pyrophosphate dipotassium salt, monohexadecyl pyrophosphate bis(triethanolamine) salt, monohexadecyl pyrophosphate tris(triethanolamine) salt, monohexadecyl tripolyphosphate dipotassium salt, monohexadecyl tripolyphosphate tripotassium salt, dihexadecyl tripolyphosphate dipotassium salt, monooctadecyl pyrophosphate monopotassium salt, monooctadecyl pyrophosphate dipotassium salt, monooctadecyl pyrophosphate Octadecyl pyrophosphate tripotassium salt, dioctadecyl pyrophosphate monopotassium salt, dioctadecyl pyrophosphate dipotassium salt, monooctadecyl pyrophosphate bis(triethanolamine) salt, monooctadecyl pyrophosphate tris(triethanolamine) salt, monooctadecyl tripolyphosphate dipotassium salt, monooctadecyl tripolyphosphate tripotassium salt, dioctadecyl tripolyphosphate dipotassium salt, monoicosyl pyrophosphate dipotassium salt, monoicosyl pyrophosphate tripotassium salt , diicosyl pyrophosphate dipotassium salt, monodocosyl pyrophosphate dipotassium salt, monodocosyl pyrophosphate tripotassium salt, didocosyl pyrophosphate dipotassium salt, mono-iso-octadecyl pyrophosphate dipotassium salt, mono-iso-octadecyl pyrophosphate tripotassium salt, di-iso-octadecyl pyrophosphate dipotassium salt, mono-2-hexyldecyl pyrophosphate dipotassium salt, di-2-hexyldecyl pyrophosphate dipotassium salt, mono-2-octyldodecyl pyrophosphate dipotassium salt,Among them, in terms of emulsion stability and fiber opening properties, monohexadecyl pyrophosphate monopotassium salt, monohexadecyl pyrophosphate dipotassium salt, monohexadecyl pyrophosphate tripotassium salt, dihexadecyl pyrophosphate dipotassium salt, monooctadecyl pyrophosphate monopotassium salt, monooctadecyl pyrophosphate dipotassium salt, monooctadecyl pyrophosphate tripotassium salt, dioctadecyl pyrophosphate dipotassium salt, mono Neuicosyl pyrophosphate dipotassium salt, monoicosyl pyrophosphate tripotassium salt, monodocosyl pyrophosphate dipotassium salt, monodocosyl pyrophosphate tripotassium salt, mono-iso-octadecyl pyrophosphate monopotassium salt, mono-iso-octadecyl pyrophosphate dipotassium salt, mono-iso-octadecyl pyrophosphate tripotassium salt, and di-iso-octadecyl pyrophosphate dipotassium salt are preferred.
[0023] [Organophosphate ester compounds having a hydrocarbon group having 14 to 22 carbon atoms other than compounds (A1), (A2), and (A3)] Compound (A) may contain an organophosphate ester compound having a hydrocarbon group having 14 to 22 carbon atoms other than compounds (A1), (A2), and (A3). The organic phosphate ester compound having a hydrocarbon group having 14 to 22 carbon atoms other than the compound (A1), the compound (A2), and the compound (A3) is not particularly limited, and examples thereof include monotetradecenyl phosphate monopotassium salt, monotetradecenyl phosphate dipotassium salt, ditetradecenyl phosphate potassium salt, monotetradecenyl pyrophosphate dipotassium salt, monohexadecenyl phosphate monopotassium salt, monohexadecenyl phosphate dipotassium salt, dihexadecenyl phosphate potassium salt, monohexadecenyl pyrophosphate dipotassium salt, monooctadecenyl phosphate monopotassium salt, monooctadecenyl phosphate dipotassium salt, dioctadecenyl phosphate potassium salt, monooctadecenyl pyrophosphate dipotassium salt, monooctadecenyl phosphate disodium salt, monooctadecenyl phosphate Examples of such phosphates include bis(triethanolamine) salt, monoicosenyl phosphate monopotassium salt, monoicosenyl phosphate dipotassium salt, diicosenyl phosphate potassium salt, monodocosenyl phosphate monopotassium salt, monodocosenyl phosphate dipotassium salt, didocosenyl phosphate potassium salt, monooctadecadienyl phosphate monopotassium salt, monooctadecadienyl phosphate dipotassium salt, dioctadecadienyl phosphate potassium salt, monononylphenyl phosphate dipotassium salt, dinonylphenyl phosphate potassium salt, tritetradecyl phosphate, trihexadecyl phosphate, trioctadecyl phosphate, triicosyl phosphate, tridocosyl phosphate, tri-isooctadecyl phosphate, trihexyldecyl phosphate, and trioctadecenyl phosphate.
[0024] [Nonionic surfactant (B)] The treatment agent for regenerated cellulose fibers of the present invention contains a nonionic surfactant (B). There are no particular limitations on the nonionic surfactant (B), but from the viewpoint of imparting the fiber bundling properties required in the spun yarn production process and the nonwoven fabric production process, it preferably contains at least one selected from the group consisting of the compound represented by the above general formula (4) and a nitrogen-containing nonionic surfactant, and more preferably contains the compound represented by the above general formula (4).
[0025] The compound represented by general formula (4) is not particularly limited, and one or more kinds may be used in combination. 6 is an alkyl group having 8 to 22 carbon atoms, an alkenyl group having 8 to 22 carbon atoms, an alkanoyl group having 8 to 22 carbon atoms, or an alkenoyl group having 8 to 22 carbon atoms. 6 Although there are no particular limitations on R, from the viewpoint of imparting fiber bundling properties required in the spun yarn production process and the nonwoven fabric production process, an alkyl group having 8 to 22 carbon atoms, an alkenyl group having 8 to 22 carbon atoms, or an alkenoyl group having 8 to 22 carbon atoms is preferred, an alkyl group having 8 to 22 carbon atoms or an alkenyl group having 8 to 22 carbon atoms is more preferred, and an alkyl group having 8 to 22 carbon atoms is even more preferred. 6 The upper limit of the number of carbon atoms is preferably 20, more preferably 18, and the lower limit of the number of carbon atoms is preferably 10, more preferably 12. Furthermore, for example, 10 to 20 is preferred, and 12 to 18 is more preferred.
[0026] R 6There are no particular limitations on the alkyl group, and examples thereof include straight-chain alkyl groups such as an n-octyl group, an n-nonyl group, an n-decyl group, an n-undecyl group, an n-dodecyl group, an n-tridecyl group, an n-tetradecyl group, an n-pentadecyl group, an n-hexadecyl group, an n-octadecyl group, an n-icosyl group, and an n-docosyl group; an iso-undecyl group, an iso-tridecyl group, an iso-tetradecyl group, an iso-pentadecyl group, an iso-hexadecyl group, an iso-octadecyl group, a 2-ethylhexyl group, a 2-propylheptyl group, a 3-propylheptyl group, a 2-butyloctyl group, a 4-butyloctyl group, a 2-hexyloctyl group, and a 2-hexyldecyl group. branched alkyl groups such as an octenyl group, a 2-octyldodecyl group, and a 3,5,5-trimethylhexyl group; alkenyl groups such as an octenyl group, a decenyl group, a dodecenyl group, an octadecenyl group, a hexadecenyl group, an octadecenyl group, an icosenyl group, and a docosenyl group; alkanoyl groups such as an octanoyl group, a decanoyl group, a dodecanoyl group, a tetradecanoyl group, a hexadecanoyl group, an octadecanoyl group, an icosanoyl group, and a docosanoyl group; and alkenoyl groups such as an octenoyl group, a decenoyl group, a dodecenoyl group, an octadecenoyl group, a hexadecenyl group, an octadecenoyl group, an icosenoyl group, and a docosenoyl group.
[0027] In formula (4), R 7 is a hydrogen atom, an alkyl group having 8 to 22 carbon atoms, an alkenyl group having 8 to 22 carbon atoms, an alkanoyl group having 8 to 22 carbon atoms, or an alkenoyl group having 8 to 22 carbon atoms. 7 Although there are no particular limitations on R, from the viewpoint of fiber bundling, a hydrogen atom, an alkyl group having 8 to 22 carbon atoms, an alkenyl group having 8 to 22 carbon atoms, or an alkenoyl group having 8 to 22 carbon atoms is preferred, an alkyl group having 8 to 22 carbon atoms or an alkenyl group having 8 to 22 carbon atoms is more preferred, and an alkyl group having 8 to 22 carbon atoms is even more preferred. 7 is other than a hydrogen atom, from the viewpoint of fiber bundling, R 7 The upper limit of the number of carbon atoms is preferably 20, more preferably 18, and the lower limit of the number of carbon atoms is preferably 10, more preferably 12. Furthermore, for example, 10 to 20 is preferred, and 12 to 18 is more preferred.
[0028] R7 is not particularly limited, and examples thereof include a hydrogen atom; a straight-chain alkyl group such as an n-octyl group, an n-nonyl group, an n-decyl group, an n-undecyl group, an n-dodecyl group, an n-tridecyl group, an n-tetradecyl group, an n-pentadecyl group, an n-hexadecyl group, an n-octadecyl group, an n-icosyl group, or an n-docosyl group; an iso-undecyl group, an iso-tridecyl group, an iso-tetradecyl group, an iso-pentadecyl group, an iso-hexadecyl group, an iso-octadecyl group, a 2-ethylhexyl group, a 2-propylheptyl group, a 3-propylheptyl group, a 2-butyloctyl group, a 4-butyloctyl group, a 2-hexyloctyl group, a 2-hexyl branched alkyl groups such as dodecyl, 2-octyldodecyl, and 3,5,5-trimethylhexyl; alkenyl groups such as octenyl, decenyl, dodecenyl, octadecenyl, hexadecenyl, octadecenyl, icosenyl, and docosenyl; alkanoyl groups such as octanoyl, decanoyl, dodecanoyl, tetradecanoyl, hexadecanoyl, octadecanoyl, icosanoyl, and docosanoyl; and alkenoyl groups such as octenoyl, decenoyl, dodecenoyl, octadecenoyl, hexadecenyl, octadecenoyl, icosenoyl, and docosenoyl.
[0029] In formula (4), a and b are each integers of 0 to 20, and satisfy 3≦a+b≦40. From the viewpoint of imparting fiber bundling properties required in the spun yarn production process and the nonwoven fabric production process, the upper limit of a is preferably 18, more preferably 15, and even more preferably 10. From the viewpoint of fiber bundling properties, the upper limit of b is preferably 18, and more preferably 15. On the other hand, the lower limit of b is preferably 3, and more preferably 5. Also, for example, 3 to 18 is preferred, and 5 to 15 is more preferred. From the viewpoint of fiber bundling properties, the upper limit of a+b is preferably 35, more preferably 30, and even more preferably 20. On the other hand, the lower limit of b is preferably 4, and more preferably 5. Also, for example, 4≦a+b≦30 is preferred, and 5≦a+b≦20 is more preferred. From the viewpoint of fiber bundling properties, a and b preferably satisfy a≦b, and even more preferably a<b. In formula (4), 3 H6 O) and (C 2 H 4 O) may be arranged randomly or in blocks.
[0030] The compound represented by the general formula (4) is not particularly limited, but examples thereof include polyoxyalkylene aliphatic alcohol ethers and polyoxyalkylene fatty acid esters.
[0031] Examples of polyoxyalkylene aliphatic alcohol ethers include, but are not limited to, EO(3)-octyl ether, EO(5)-decyl ether, EO(5)-dodecyl ether, EO(15)-dodecyl ether, EO(7)-tetradecyl ether, EO(8)-hexadecyl ether, EO(10)-octadecyl ether, EO(10)-octadecenyl ether, EO(20)-octadecenyl ether, EO(12)-icosyl ether, EO(13)-octadecenyl ether, EO(14)-octadecenyl ether, EO(15)-octadecenyl ether, EO(16)-octadecenyl ether, EO(17)-octadecenyl ether, EO(18)-octadecenyl ether, EO(19)-octadecenyl ether, EO(20)-octadecenyl ether, EO(21)-octadecenyl ether, EO(22)-octadecenyl ether, EO(23)-octadecenyl ether, EO(24)-octadecenyl ether, EO(25)-octadecenyl ether, EO(26)-octadecenyl ether, EO(27)-octadecenyl ether, EO(28)-octadecenyl ether, EO(29)-octadecenyl ether, EO(30)-octadecenyl ether, EO(31)-octadecenyl ether, EO(32)-octadecenyl ether, EO(33)-octadecenyl ether, EO(34)-octadecenyl ether, EO(35)-octadecenyl ether, EO(36)-octadecenyl ether O(15)-docosyl ether, EO(5)-iso-dodecyl ether, EO(10)-iso-octadecyl ether, EO(4)-2-ethylhexyl ether, EO(5)-2-butyloctyl ether, EO(8)-2-hexyldecyl ether, PO(10)-dodecyl ether, PO(5)-2-ethylhexyl ether, PO(1) / EO(4)-octyl ether, PO(10) / EO(20)-octyl ether, PO(2) / EO(5)-decyl ether, PO(3) / EO(5)-dodecyl ether, PO(7) / EO(3)-dodecyl ether, PO(4) / EO(7)-tridecyl ether, PO(4) / EO(8)-tetradecyl ether, PO(5) / EO(8)-hexadecyl ether, PO(5) / EO(10)-octadecyl ether, PO(15) / EO(15)-octadecyl ether, PO(10) / EO(10)-octadecenyl ether, PO(2) / EO(6)-iso-dodecyl ether ethyl ether, PO(2) / EO(6)-iso-tridecyl ether, PO(4) / EO(8)-iso-hexadecyl ether, PO(5) / EO(15)-iso-octadecyl ether, PO(3) / EO(3)-2-ethylhexyl ether, PO(2) / EO(6)-2-butyloctyl ether, PO(1) / EO(6)-3,5,5-trimethylhexyl ether, PO(15) / EO(10)-di-2-ethylhexyl ether, etc. In the above, EO represents ethylene oxide, PO represents propylene oxide, and the numbers in parentheses represent the number of moles of each alkylene oxide added.For example, EO(5) means that 5 moles of ethylene oxide are added, and PO(1) / EO(4) means that 1 mole of propylene oxide and 4 moles of ethylene oxide are added.
[0032] The polyoxyalkylene fatty acid ester refers to an ester having a structure in which a hydroxyl group of a polyalkylene glycol and a monovalent fatty acid are esterified. Examples of the polyoxyalkylene fatty acid ester include, but are not limited to, polyoxyethylene (3 to 40 mol) laurate, polyoxyethylene (3 to 40 mol) dilaurate, polyoxyethylene (3 to 40 mol) palmitate, polyoxyethylene (3 to 40 mol) dipalmitate, polyoxyethylene (3 to 40 mol) stearate, polyoxyethylene (3 to 40 mol) distearate, polyoxyethylene (3 to 40 mol) oleate, polyoxyethylene (3 to 40 mol) dioleate, polyoxyethylene (3 to 40 mol) itaconate, polyoxyethylene (3 to 40 mol) behenate, polyoxypropylene (3 to 40 mol) laurate, and PO(10) / EO(20)-oleate.
[0033] The nitrogen-containing nonionic surfactant is not particularly limited as long as it is a nonionic surfactant containing a nitrogen atom, but examples include those having a structure in which 2 to 100 moles of alkylene oxide having 2 to 3 carbon atoms are added to 1 mole of organic amine. The organic amine is not particularly limited, but examples include organic amines having a monovalent hydrocarbon group having 8 to 22 carbon atoms. From the viewpoint of imparting the fiber bundling properties required in the spun yarn production process and the nonwoven fabric production process, the upper limit of the carbon number is preferably 20, more preferably 18. Meanwhile, the lower limit of the carbon number is preferably 10, more preferably 12. Furthermore, for example, 10 to 20 is preferred, more preferably 12 to 18. The hydrocarbon group contained in the organic amine may be a saturated hydrocarbon group, an unsaturated hydrocarbon group, a linear hydrocarbon group, or a branched hydrocarbon group. The alkylene oxide having 2 to 3 carbon atoms is preferably at least one selected from ethylene oxide and propylene oxide. From the viewpoint of fiber bundling ability, the upper limit of the number of moles of alkylene oxide added is preferably 50 moles, more preferably 30 moles, and even more preferably 20 moles. On the other hand, the lower limit of the number of moles is preferably 3 moles, more preferably 4 moles, and even more preferably 5 moles. Also, for example, 3 moles to 50 moles is preferable, and 5 moles to 20 moles is more preferable.
[0034] The linear saturated hydrocarbon group is not particularly limited, but examples thereof include an octyl group, a nonyl group, a decyl group, an undecyl group, a dodecyl group, a tridecyl group, a tetradecyl group, a pentadecyl group, a hexadecyl group, a heptadecyl group, an octadecyl group, an icosyl group, and a docosyl group.
[0035] Examples of saturated hydrocarbon groups having a branched chain structure include an iso-octyl group, an iso-nonyl group, an iso-decyl group, an iso-undecyl group, an iso-dodecyl group, an iso-tridecyl group, an iso-tetradecyl group, an iso-hexadecyl group, an iso-octadecyl group, an iso-icosyl group, an iso-docosyl group, a 2-ethylhexyl group, a 2-butyloctyl group, a 2-hexyldecyl group, and a 2-octyldodecyl group.
[0036] The unsaturated hydrocarbon group may be an alkenyl group having one double bond as an unsaturated carbon bond, or an alkadienyl group or alkatrienyl group having two or more double bonds. Furthermore, the unsaturated hydrocarbon group may be an alkynyl group having one triple bond as an unsaturated carbon bond, or an alkadiynyl group having two or more triple bonds. Specific examples of linear unsaturated hydrocarbon groups having one double bond in the hydrocarbon group include octenyl, nonenyl, decenyl, undecenyl, dodecenyl, tridecenyl, tetradecenyl, pentadecenyl, hexadecenyl, heptadecenyl, octadecenyl, icosenyl, and docosenyl.
[0037] Specific examples of the unsaturated hydrocarbon group having a branched chain structure and one double bond in the hydrocarbon group include an iso-octenyl group, an iso-nonenyl group, an iso-decenyl group, an iso-undecenyl group, an iso-dodecenyl group, an iso-tridecenyl group, an iso-tetradecenyl group, an iso-hexadecenyl group, an iso-octadecenyl group, an iso-icosenyl group, and an iso-docosenyl group.
[0038] Specific examples of organic amines include octylamine, nonylamine, decylamine, dodecylamine, tetradecylamine, hexadecylamine, octadecylamine, icosylamine, docosylamine, decenylamine, dodecenylamine, tetradecenylamine, hexadecenylamine, octadecenylamine, iso-octylamine, iso-tridecylamine, iso-octadecylamine, 2-ethylhexylamine, and 2-octyldodecylamine.
[0039] The nonionic surfactant other than the compound represented by general formula (4) and the nitrogen-containing nonionic surfactant is not particularly limited, but preferred are ester compounds having a structure in which a polyhydric alcohol and a fatty acid are ester-bonded and having one or more hydroxyl groups in the molecule (hereinafter simply referred to as ester compounds having one or more hydroxyl groups in the molecule), polyoxyalkylene sorbitan fatty acid esters, polyoxyalkylene castor oil ethers, polyoxyalkylene hydrogenated castor oil ethers, polycarboxylic acid esters, and the like.
[0040] The ester compound having one or more hydroxyl groups in the molecule has a structure in which a polyhydric alcohol and a fatty acid are ester-bonded, and has one or more hydroxyl groups in the molecule.
[0041] The polyhydric alcohol that is a constituent element of the ester compound having one or more hydroxyl groups in the molecule is not particularly limited, but sorbitan and glycerin are preferred in terms of emulsion stability. The fatty acid that is a constituent element of the ester compound having one or more hydroxyl groups in the molecule is not particularly limited, but saturated and / or unsaturated fatty acids having 12 to 18 carbon atoms are preferred in terms of emulsion stability.
[0042] The ester compound having one or more hydroxyl groups in the molecule is not particularly limited, but from the viewpoint of emulsion stability, sorbitan monoester, sorbitan diester, sorbitan triester, glycerin monoester, and glycerin diester are preferred, and sorbitan monoester is more preferred. Examples of sorbitan monoesters include sorbitan monostearate, sorbitan monooleate, sorbitan monopalmitate, and sorbitan monolaurate. Examples of sorbitan diesters include sorbitan distearate, sorbitan dioleate, sorbitan dipalmitate, and sorbitan dilaurate. Examples of sorbitan triesters include sorbitan tristearate, sorbitan trioleate, sorbitan tripalmitate, and sorbitan trilaurate. Examples of glycerin monoesters include glycerin monostearate and glycerin monooleate. Examples of glycerin diesters include glycerin distearate, glycerin dioleate, glycerin dipalmitate, and glycerin dilaurate.
[0043] Polyoxyalkylene sorbitan fatty acid esters are compounds having a structure in which an alkylene oxide such as ethylene oxide, propylene oxide, or butylene oxide is added to a sorbitan fatty acid monoester, a sorbitan fatty acid diester, or a sorbitan fatty acid triester. The polyoxyalkylene sorbitan fatty acid ester is not particularly limited, but examples thereof include polyoxyethylene (1 to 25 mol) sorbitan monostearate, polyoxyethylene (1 to 25 mol) sorbitan monooleate, polyoxyethylene (1 to 25 mol) sorbitan monopalmitate, polyoxyethylene (1 to 25 mol) sorbitan monolaurate, polyoxyethylene (1 to 25 mol) sorbitan distearate, polyoxyethylene (1 to 25 mol) sorbitan dioleate, polyoxyethylene (1 to 25 mol) sorbitan dipalmitate, polyoxyethylene (1 to 25 mol) sorbitan dilaurate, polyoxyethylene (1 to 25 mol) sorbitan tristearate, polyoxyethylene (1 to 25 mol) sorbitan trioleate, sorbitan tripalmitate, and polyoxyethylene (1 to 25 mol) sorbitan trilaurate.
[0044] Polyoxyalkylene castor oil ethers are compounds having a structure in which alkylene oxides such as ethylene oxide, propylene oxide, and butylene oxide are added to castor oil. Examples of polyoxyalkylene castor oil ethers include, but are not limited to, polyoxyethylene castor oil ether (polyoxyethylene (1 to 25 moles) castor oil ether).
[0045] Polyoxyalkylene hydrogenated castor oil ether is a compound having a structure in which an alkylene oxide such as ethylene oxide, propylene oxide, or butylene oxide is added to hydrogenated castor oil. The polyoxyethylene hydrogenated castor oil ether is not particularly limited, but examples thereof include polyoxyethylene hydrogenated castor oil ether (polyoxyethylene (1 to 25 moles) hydrogenated castor oil ether).
[0046] Polycarboxylic acid esters are compounds having a structure in which a polycarboxylic acid and a polyol are ester-bonded. The polycarboxylic acid is preferably a divalent or higher carboxylic acid having 10 to 66 carbon atoms. Examples of polycarboxylic acids include sebacic acid, oleic acid dimer, erucic acid dimer, oleic acid trimer, and erucic acid trimer. Among polycarboxylic acids, dimer acids of unsaturated fatty acids having 18 to 22 carbon atoms are preferred, and dimer acids of unsaturated fatty acids having 18 carbon atoms are more preferred. The polycarboxylic acid may be an aliphatic polycarboxylic acid or an aromatic polycarboxylic acid, and is preferably an aliphatic polycarboxylic acid. The polyol is a divalent or higher alcohol having an oxyalkylene group having 2 to 3 carbon atoms in the molecule. The polyol is not particularly limited as long as it is a dihydric or higher alcohol and has a (poly)oxyalkylene group in the molecule, but examples thereof include polyalkylene glycols composed of oxyethylene units and / or oxypropylene units, polyoxyalkylene sorbitan, polyoxyalkylene sorbitan fatty acid esters, polyoxyalkylene glycerin, polyoxyalkylene polyglycerin, polyoxyalkylene polyglycerin esters, etc. Among these, polyalkylene glycols composed of oxyethylene units and / or oxypropylene units are preferred. Examples of polyalkylene glycols composed of oxyethylene units and / or oxypropylene units include polyoxyethylene glycol, polypropylene glycol, polyoxyethylene polyoxypropylene glycol, etc. Polyoxyethylene polyoxypropylene glycol may be a block or random product. Examples of polyalkylene glycols composed of oxyethylene units and / or oxypropylene units include polyoxyethylene glycol. The number average molecular weight of the polyalkylene glycol is preferably 100 to 10,000, more preferably 200 to 2,000, and even more preferably 400 to 1,000.
[0047] [Inorganic Phosphate (Salt)] From the viewpoint of antistatic properties, the treating agent for regenerated cellulose fibers of the present invention preferably contains inorganic phosphoric acid (salt). The inorganic phosphoric acid (salt) is at least one selected from phosphoric acid, metal dihydrogen phosphate, dimetal hydrogen phosphate, and trimetal phosphate. Specific examples of the monometal dihydrogen phosphate include monopotassium dihydrogen phosphate and monosodium dihydrogen phosphate. Examples of the dimetal hydrogen phosphate include dipotassium hydrogen phosphate and disodium hydrogen phosphate. Examples of the trimetal phosphate include tripotassium phosphate and trisodium phosphate.
[0048] [Other Components] The regenerated cellulose fiber treatment agent of the present invention may contain anionic surfactants, amphoteric surfactants, and modified silicones as other components in order to achieve the effects of the present invention. The anionic surfactant is not particularly limited, but alkyl sulfate salts, alkyl sulfonate salts, dialkyl sulfosuccinate salts, and the like are preferred. Examples of alkyl sulfate salts include alkyl sulfate salts having a structure obtained by sulfating and neutralizing a polyhydric alcohol fatty acid ester. The sulfation method is not particularly limited, and known methods using fuming sulfuric acid, concentrated sulfuric acid, chlorosulfonic acid, sulfur trioxide gas, and the like can be used. The neutralization method is not particularly limited, and known methods can be used. Examples of basic substances used for neutralization include alkali metal carbonates such as sodium carbonate and potassium carbonate, alkali metal bicarbonates such as sodium bicarbonate and potassium bicarbonate, alkali metal hydroxides such as sodium hydroxide, potassium hydroxide, and lithium hydroxide, alkaline earth metal oxides and hydroxides such as calcium oxide, calcium hydroxide, magnesium oxide, and magnesium hydroxide, ammonia, mono-, di-, and trialkanolamines having 2 to 4 carbon atoms in the hydroxyalkyl chain, and primary, secondary, and tertiary alkylamines having 1 to 4 carbon atoms in the alkyl chain. Two or more basic substances may be used in combination. The fatty acid used in the synthesized polyhydric alcohol fatty acid ester product essentially contains an unsaturated fatty acid and may also contain saturated fatty acids, hydroxy fatty acids, or hydroxy unsaturated fatty acids. Preferred alkyl sulfate salts are polyhydric alcohol fatty acid ester sulfate salts. Dialkyl sulfosuccinate salts are dialkyl esters of succinic acid having a sulfonate group at the α-position. The alkyl group constituting the dialkyl ester preferably has 6 to 18 carbon atoms. The upper limit of the alkyl group is more preferably 16, further preferably 14, and particularly preferably 13. On the other hand, the lower limit of the alkyl group is more preferably 7, further preferably 8, and particularly preferably 9. Furthermore, for example, 8 to 18 are more preferable, and 10 to 13 are more preferable.
[0049] [Treatment Agent for Regenerated Cellulose Fibers] The treatment agent for regenerated cellulose fibers of the present invention contains the above-mentioned organic phosphate ester compound (A) and the above-mentioned nonionic surfactant (B), and the weight ratio (A / B) of the organic phosphate ester compound (A) to the nonionic surfactant (B) is 0.05 to 1.0. The reason why the treatment agent for regenerated cellulose fibers of the present invention has excellent nep suppression properties is not particularly limited, but it is believed that the high melting point of the organic phosphate ester compound (A) provides excellent fiber opening properties, while the nonionic surfactant (B) provides adequate fiber bundling properties, thereby suppressing fiber entanglement and promoting the disentanglement of entanglements during processing due to the interaction between fibers, thereby suppressing defects such as bundling and neps. If the proportion of compound (A) is low and the (A / B) ratio is less than 0.05, smoothness is insufficient, entanglement cannot be suppressed, and nep suppression properties are reduced. On the other hand, if the proportion of compound (A) is large and (A / B) exceeds 1.0, the fiber bundling ability will be insufficient, and the resulting entanglements may not be untangled, resulting in a decrease in nep suppression ability. In addition, the shape stability of the fiber assembly during the processing step will be insufficient, resulting in a decrease in the uniformity of the spun yarn or nonwoven fabric.
[0050] The acid value of the nonvolatile content of the treatment agent of the present invention is preferably 0.1 to 70 mgKOH / g in terms of emulsion stability and foam suppression. The upper limit of the acid value is preferably 60 mgKOH / g, more preferably 55 mgKOH / g, and even more preferably 50 mgKOH / g. On the other hand, the lower limit of the acid value is preferably 0.5 mgKOH / g, more preferably 1 mgKOH / g, and even more preferably 3 mgKOH / g in terms of foam suppression. Also, for example, 0.5 to 60 mgKOH / g is preferable, more preferably 1 to 55 mgKOH / g, and even more preferably 3 to 50 mgKOH / g is preferable. The nonvolatile content of the water permeability imparting agent in the present invention refers to the residue on the aluminum sheet when 2.0 to 3.0 g of the imparting agent is spread evenly on an aluminum sheet, dried at 110°C under infrared lamp irradiation, and the fluctuation range of the volatile content over 150 seconds reaches 0.15%.
[0051] The weight ratio (A / B) of the compound (A) to the surfactant (B) is not particularly limited as long as it is 0.05 to 1.0, but from the viewpoint of imparting defibration properties without impairing fiber bundling properties, the upper limit of the weight ratio is preferably 0.9, more preferably 0.8, and even more preferably 0.7, and the lower limit of the weight ratio is preferably 0.08, more preferably 0.11, and even more preferably 0.15. Also, for example, the range is preferably 0.08 to 0.9, and more preferably 0.15 to 0.7.
[0052] The proportion of compound (A) in the nonvolatile content of the treatment agent of the present invention is not particularly limited, but from the viewpoint of imparting defibration properties without impairing fiber bundling properties, it is preferably 5 to 50 wt%. The upper limit of this proportion is more preferably 45 wt%, even more preferably 40 wt%, and particularly preferably 35 wt%. Meanwhile, the lower limit of this proportion is more preferably 8 wt%, even more preferably 10 wt%, and particularly preferably 15 wt%. Furthermore, for example, 8 to 45 wt% is more preferable, and 15 to 35 wt% is even more preferable.
[0053] The proportion of compound (A1) in compound (A) of the treatment agent of the present invention is not particularly limited, but from the viewpoint of imparting smoothness, it is preferably 1 to 60 wt %. The upper limit of this proportion is more preferably 55 wt %, and particularly preferably 50 wt %. Meanwhile, the lower limit of this proportion is more preferably 5 wt %, and particularly preferably 10 wt %. Furthermore, for example, 5 to 55 wt % is more preferable, and 10 to 50 wt % is even more preferable.
[0054] The proportion of compound (A2) in compound (A) of the treatment agent of the present invention is not particularly limited, but from the viewpoint of imparting smoothness, it is preferably 1 to 70 wt %. The upper limit of this proportion is more preferably 60 wt %, and particularly preferably 55 wt %. Meanwhile, the lower limit of this proportion is more preferably 10 wt %, and particularly preferably 15 wt %. Furthermore, for example, 10 to 60 wt % is more preferable, and 15 to 55 wt % is even more preferable.
[0055] Compound (A) is R 1 is a monovalent saturated hydrocarbon group having 16 to 22 carbon atoms; and 2 and R 3is preferably at least one compound selected from the compounds represented by the general formula (2) in which R is independently a monovalent saturated hydrocarbon group having 16 to 22 carbon atoms, in terms of fiber-opening properties, 1 is a monovalent saturated hydrocarbon group having 16 to 22 carbon atoms; and 2 and R 3 are each independently a monovalent saturated hydrocarbon group having 16 to 22 carbon atoms.
[0056] R in the compound (A) of the treating agent of the present invention 1 The proportion of the compound represented by general formula (1), in which is a monovalent saturated hydrocarbon group having 16 to 22 carbon atoms, is not particularly limited, but is preferably 5 to 60% by weight from the viewpoint of fiber-opening properties. The upper limit of this proportion is more preferably 55% by weight, even more preferably 50% by weight, and particularly preferably 45% by weight. On the other hand, the lower limit of this proportion is more preferably 10% by weight, even more preferably 15% by weight, and particularly preferably 20% by weight. Also, for example, 10 to 55% by weight is more preferable, 15 to 50% by weight is more preferable, and 20 to 45% by weight is particularly preferable.
[0057] R in the compound (A) of the treating agent of the present invention 2 and R 3 are each independently a monovalent saturated hydrocarbon group having 16 to 22 carbon atoms. The proportion of the compound represented by general formula (2) is not particularly limited, but from the viewpoint of fiber-opening property, it is preferably 10 to 70% by weight. The upper limit of this proportion is more preferably 65% by weight, even more preferably 60% by weight, and particularly preferably 55% by weight. On the other hand, the lower limit of this proportion is more preferably 15% by weight, even more preferably 20% by weight, and particularly preferably 25% by weight. Also, for example, it is more preferably 15 to 65% by weight, even more preferably 20 to 60% by weight, and particularly preferably 25 to 55% by weight.
[0058] The proportion of compound (A3) in compound (A) of the treatment agent of the present invention is not particularly limited, but from the viewpoint of imparting smoothness, it is preferably 0 to 70 wt %. The upper limit of this proportion is more preferably 60 wt %, and particularly preferably 55 wt %. On the other hand, the lower limit of this proportion is more preferably 5 wt %, and particularly preferably 10 wt %. Furthermore, for example, 5 to 60 wt % is more preferable, and 10 to 55 wt % is even more preferable.
[0059] The weight ratio of compound (A1) to the total of compound (A1) and compound (A2) (A1 / (A2+A2)) is not particularly limited, but from the viewpoint of imparting smoothness, it is preferably 0.01 to 0.6. The upper limit of this weight ratio is more preferably 0.55, and particularly preferably 0.5. On the other hand, the lower limit of this weight ratio is more preferably 0.15, and particularly preferably 0.3. Furthermore, for example, it is more preferably 0.15 to 0.55, and even more preferably 0.3 to 0.5.
[0060] The weight ratio of compound (A1) to the total of compound (A1), compound (A2), and compound (A3) (A1 / (A1+A2+A3)) is not particularly limited, but from the viewpoint of imparting smoothness, it is preferably 0.01 to 0.6. The upper limit of this weight ratio is more preferably 0.5, and particularly preferably 0.4. On the other hand, the lower limit of this weight ratio is more preferably 0.1, and particularly preferably 0.15. Furthermore, for example, it is more preferably 0.1 to 0.5, and even more preferably 0.15 to 0.4.
[0061] The proportion of the nonionic surfactant (B) in the nonvolatile content of the treatment agent of the present invention is not particularly limited, but from the viewpoint of imparting appropriate fiber bundling properties, it is preferably 50 to 95% by weight. The upper limit of this proportion is more preferably 90% by weight, and particularly preferably 85% by weight. Meanwhile, the lower limit of this proportion is more preferably 55% by weight, and particularly preferably 60% by weight. Furthermore, for example, 55 to 90% by weight is more preferable, and 60 to 85% by weight is even more preferable.
[0062] The proportion of at least one selected from the compound represented by formula (4) and the nitrogen-containing nonionic surfactant in the nonvolatile content of the treatment agent of the present invention is not particularly limited, but from the viewpoint of imparting appropriate fiber bundling properties, it is preferably 20 to 95 wt%. The upper limit of this proportion is more preferably 90 wt%, and particularly preferably 85 wt%. Meanwhile, the lower limit of this proportion is more preferably 30 wt%, and particularly preferably 50 wt%. Furthermore, for example, 30 to 90 wt% is more preferable, and 50 to 85 wt% is even more preferable.
[0063] The proportion of inorganic phosphoric acid (salt) in the nonvolatile content of the treatment agent of the present invention is not particularly limited, but is preferably 0.01 to 3 wt % in terms of antistatic properties and suppression of moisture absorption. The upper limit of this proportion is more preferably 2 wt %, and particularly preferably 1 wt %. Meanwhile, the lower limit of this proportion is more preferably 0.02 wt %, and particularly preferably 0.03 wt %. Furthermore, for example, 0.01 to 2 wt % is more preferable, and 0.02 to 1 wt % is even more preferable.
[0064] [Treatment Agent for Regenerated Cellulose Fibers Consisting of Multiple Treatment Agent Sets, Multi-Component First Treatment Agent for Regenerated Cellulose Fibers, and Multi-Component Second Treatment Agent for Regenerated Cellulose Fibers] The treatment agent for regenerated cellulose fibers of the present invention may be a multi-component treatment agent composed of multiple treatment agent sets. A treatment agent for regenerated cellulose fibers composed of multiple treatment agent sets is a treatment agent composed of multiple treatment agent sets including a multi-component first treatment agent for regenerated cellulose fibers containing compound (A) and a multi-component second treatment agent for regenerated cellulose fibers containing nonionic surfactant (B), as long as these are applied to regenerated cellulose fibers so that the organic phosphate ester compound (A) and the nonionic surfactant (B) meet the specific weight ratio of the present invention. By making the treatment agent of the present invention a multi-component treatment agent, the storage stability of each of the organic phosphate ester compound (A) and the nonionic surfactant (B) can be improved, thereby providing stable nep suppression to regenerated cellulose fibers. When used as a multi-component treatment agent, the treatment agent for regenerated cellulose fibers, the multi-component first treatment agent for regenerated cellulose fibers, and the multi-component second treatment agent for regenerated cellulose fibers, which are composed of a multiple treatment agent set of the present invention, exhibit excellent nep suppression properties by having the organic phosphate ester compound (A) and the nonionic surfactant (B) on the regenerated cellulose fibers in the specific weight ratio of the present invention.
[0065] <Method for manufacturing a treatment agent for regenerated cellulose fibers, a treatment agent for regenerated cellulose fibers consisting of a set of multiple treatment agents, a multi-component first treatment agent for regenerated cellulose fibers, and a multi-component second treatment agent for regenerated cellulose fibers> The treatment agent for regenerated cellulose fibers of the present invention can be manufactured by mixing compound (A) and nonionic surfactant (B), as well as other components as necessary, and there is no particular limitation on the order in which the components are mixed, and known methods can be used.
[0066] There are no particular limitations on the weight percentage of water and nonvolatile matter in the treatment agent for regenerated cellulose fibers. These may be appropriately determined taking into consideration factors such as the transportation costs of the treatment agent of the present invention and the ease of handling due to the emulsion viscosity. The weight percentage of water in the entire treatment agent for regenerated cellulose fibers is preferably 0.1 to 99.9 wt%, more preferably 1 to 99 wt%, and particularly preferably 2 to 95 wt%. The weight percentage (concentration) of nonvolatile matter in the entire treatment agent for regenerated cellulose fibers is preferably 0.1 to 99.9 wt%. The upper limit of this percentage is more preferably 99 wt%, and even more preferably 98 wt%. Meanwhile, the lower limit of this percentage is more preferably 1 wt%, and even more preferably 5 wt%. Furthermore, for example, 1 to 99 wt% is more preferably, and 5 to 98 wt% is even more preferably.
[0067] When the treatment agent for regenerated cellulose fibers is composed of a set of multiple treatment agents, the weight percentage of water in each of the multi-component first treatment agent for regenerated cellulose fibers containing compound (A) and the multi-component second treatment agent for regenerated cellulose fibers containing nonionic surfactant (B) is preferably 0 to 90% by weight, more preferably 0 to 80% by weight, and particularly preferably 0 to 70% by weight. The weight percentage (concentration) of nonvolatile matter in each of the first treatment agent and the second treatment agent is preferably 1 to 99% by weight, more preferably 3 to 90% by weight, and particularly preferably 5 to 80% by weight, for the first treatment agent, and is preferably 1 to 100% by weight, more preferably 3 to 99.95% by weight, and particularly preferably 5 to 99.9% by weight for the second treatment agent.
[0068] [Regenerated Cellulose Fibers] The regenerated cellulose fibers of the present invention are obtained by applying the above-mentioned treatment agent to the regenerated cellulose fiber body. The regenerated cellulose fibers of the present invention may be short or long fibers, and short fibers are preferred in that they provide better product quality improvement through nep suppression. The adhesion rate of the non-volatile content of the treatment agent to the fiber body is not particularly limited, but in terms of antistatic properties and openability, it is preferably 0.03 to 2 wt % of the cellulose fiber body, and more preferably 0.1 to 1 wt %.
[0069] The fiber body is not particularly limited as long as it is a regenerated cellulose fiber, and examples thereof include viscose rayon fiber, tenacity rayon fiber, high tenacity rayon fiber, high wet elasticity rayon fiber, cuprammonium rayon fiber, solvent spun cellulose fiber, polynosic fiber, etc.
[0070] The regenerated cellulose fibers of the present invention can be used for spinning, nonwoven fabrics, special papers, etc., with spinning being preferred because uniformity is more important.
[0071] [Method of Applying a Treating Agent for Regenerated Cellulose Fibers] The regenerated cellulose fiber treating agent of the present invention may be applied to the raw regenerated cellulose fiber body without dilution, or it may be diluted with water or the like to a concentration such that the total weight percentage of nonvolatile matter is 0.01 to 10% by weight, and then applied to the raw regenerated cellulose fiber body as a diluted solution such as an emulsion. When the regenerated cellulose fiber treating agent of the present invention is used as a multi-agent treating agent set, the treating agent set can be applied to the raw regenerated cellulose fiber body by mixing all or part of the treating agent set and applying it to the fiber immediately before application to the fiber, or by applying each treating agent comprising the treating agent set separately to the fiber. The process of applying the regenerated cellulose fiber treating agent to the raw regenerated cellulose fiber body may be any process, such as spinning, drawing, cutting, crimping, or refining of the raw regenerated cellulose fiber body. The means for applying the regenerated cellulose fiber treating agent of the present invention to the raw regenerated cellulose fiber body are not particularly limited, and methods such as roller oiling, spray oiling, and dip oiling may be used. A method that can achieve the desired adhesion rate more uniformly and efficiently can be adopted depending on the manufacturing process and characteristics of the regenerated cellulose fiber. Drying methods that can be used include drying with hot air or infrared rays, and drying by contact with a heat source.
[0072] [Production of Spun Yarn] When the regenerated cellulose fibers of the present invention are used for spun yarn, even when the carding, drawing, roving, and fine spinning processes are performed at high speeds, the excellent opening properties prevent entanglement of the fibers, resulting in good nep suppression. Furthermore, the moderate smoothness and fiber bundling properties result in good draftability. Therefore, a spun yarn with high uniformity and good quality can be obtained. Spinning processes typically include carding, drawing, and fine spinning, and spun yarn is produced from staple fibers through these processes. These processes are not particularly limited, and known methods can be used. Here, we will briefly explain the spinning process in which staple fibers treated with the regenerated cellulose fiber treatment agent of the present invention are used for spinning.
[0073] <Carding Process> The staple fibers treated with the treatment agent are untangled (opened) into fiber masses, and then combed to remove ultrashort fibers and unopened portions, etc., to form a sliver (or a web in the case of nonwoven fabric), which is then placed in a can using a coiling device (in the case of nonwoven fabric, the sliver is advanced to the next process in the form of a web). Use of the treatment agent of the present invention has the advantage of suppressing neps in the finished sliver or web, thereby reducing defects.
[0074] <Drawing Process> The obtained carded sliver is stretched to increase the parallelism of the fibers, thereby increasing the sliver strength and uniforming the sliver diameter. The resulting sliver is placed in a can, as in the carding process. The drawing process is usually repeated two to three times. Use of the treatment agent of the present invention has the advantages of good nep suppression and draftability, and high uniformity of the spun yarn.
[0075] <Spinning Process> Typical processes for producing spun yarn include ring spinning, open-end spinning, and whirling air spinning (MVS). In ring spinning, a drawn sliver is lightly twisted and stretched prior to spinning to produce a string-like roving (roving), which is then further twisted and stretched to produce a spun yarn. The resulting spun yarn is wound onto a bobbin by utilizing the difference in peripheral speed between the spindle and the traveler. The use of the treatment agent of the present invention has the advantage of suppressing defects due to neps and yarn unevenness caused by poor draftability. In open-end spinning, the drawn sliver is first unraveled with a combing wire, and the fibers are bound and twisted by the centrifugal force of a rotor rotating at high speed to produce a spun yarn. The use of the treatment agent of the present invention has the advantage of suppressing yarn unevenness caused by neps and poor fiber opening, even when the open-end spinning process is performed at a high speed. In the case of whirling air spinning, a drawn sliver is stretched and drafted to the required number of fibers, and then supplied to a whirling air spinning machine, where the swirling air flow in the machine causes the supplied fiber bundle to rotate while reversing the fiber ends around the region of the spindle tip, thereby twisting it spirally to form a spun yarn. The use of the fiber treating agent of the present invention has the advantage that yarn unevenness due to neps and poor fiber opening can be suppressed even when the whirling air spinning process is increased in speed.
[0076] <Blended Spinning> When producing spun yarn, natural fibers such as hemp, wool, cotton, and bleached cotton fibers; semi-synthetic fibers such as acetate and triacetate fibers; and synthetic fibers such as polyolefin fibers, polyester fibers, polyamide fibers, acrylic fibers, polyurethane fibers, polyvinyl chloride fibers, polyphenylene sulfide fibers, and composite fibers made of two or more thermoplastic resins can be mixed and used as needed within the range that does not impair the effects of the present invention. Examples of polyamide fibers include 6-nylon fiber, 6,6-nylon fiber, and aromatic polyamide fiber.
[0077] The present invention will be described below with reference to examples, but is not limited to these. The evaluation items and evaluation methods for each example and comparative example are as follows. The details of the treatment agents used in each example and comparative example and the evaluation results are summarized in Tables 1 to 3. In the tables, the blending ratios are all in weight percent unless otherwise specified.
[0078] [Measurement of the weight ratio (A1 / (A1+A2+A3)) in the organic phosphate ester compound (A)] The ratio of the compound (A1), the compound (A2), the compound (A3) and inorganic phosphoric acid in the organic phosphate ester compound (A) was measured by 31 Approximately 150 mg of the nonvolatile content of the measurement sample was weighed into an NMR sample tube with a diameter of 5 mm, and approximately 0.5 mL of heavy water (D 2 O) or deuterated chloroform (CDCl 3 ) was added and dissolved, and the mixture was measured using a 31P-NMR spectrometer (AVANCE400, 162 MHz, manufactured by BRUKER) and a JNM-ECZ400R, 162 MHz, manufactured by JEOL Ltd. The phosphorus peaks derived from compound (A1), compound (A2), and inorganic phosphoric acid were all detected at +4 to -1 ppm, and were assigned in the following order from the low magnetic field: inorganic phosphoric acid, compound (A1), and compound (A2). On the other hand, the phosphorus peak derived from compound (A3) was detected at -5 to -15 ppm. After the assignment, the ratios of compound (A1), compound (A2), compound (A3), and inorganic phosphoric acid were calculated from the integral ratios, and the weight ratio of compound (A1) was calculated based on the formula (A1 / (A1+A2+A3)).
[0079] [Method for Measuring Acid Value] The acid value (x mgKOH / g) referred to in the present invention was measured by the following method. The nonvolatile content of each treatment agent was used as a measurement sample, and 1 g of each sample was dissolved in 50 mL of a xylene / ethanol = 1 / 1 solution containing 0.01% phenolphthalein. A 0.1 mol / L potassium hydroxide ethanol solution was added dropwise to the solution, and the amount of liquid (y mL) required to turn a faint red color was measured, and the acid value was calculated using the following formula: x = y × 5.61
[0080] [Organophosphate ester compounds] The methods for producing the organic phosphate ester compounds P-1-1 to P-5-1 and p-1 to p-2 used in the examples and comparative examples are described below. The components obtained by the production methods for P-1-1 to P-5-1 and p-1 to p-2 are as shown in Tables 4 to 8, and the obtained organic phosphate ester compounds and inorganic phosphoric acids (salts) were mixtures of their respective unneutralized products with alkali metal salts and / or organic amine salts.
[0081] (Method for producing P-1-1) 193 g of n-tetradecyl alcohol was added to a 500 mL four-neck flask, and 54.1 g of tetraphosphorus decanoate was gradually added thereto while stirring, resulting in a reaction to obtain an unneutralized product. 357 g of ion-exchanged water and 96 g of a 50% weight concentration aqueous potassium hydroxide solution were charged into a 1-liter flask, and the unneutralized product was gradually added thereto while stirring, resulting in a partially neutralized product with a nonvolatile content of 40%.
[0082] (Method for producing P-2-1) 210 g of n-hexadecyl alcohol was added to a 500 mL four-neck flask, and while stirring, 43.8 g of tetraphosphorus hexaoxide was gradually added and reacted to obtain an unneutralized product. 367 g of ion-exchanged water and 79 g of a 50% weight concentration aqueous potassium hydroxide solution were charged into a 1-liter flask, and the unneutralized product was gradually added while stirring to obtain a partially neutralized product with a non-volatile content of 40%. (Method for producing P-2-2) 212 g of n-hexadecyl alcohol was added to a 500 mL four-neck flask, and while stirring, 42.3 g of tetraphosphorus hexaoxide was gradually added and reacted to obtain an unneutralized product. 370 g of ion-exchanged water and 76 g of a 50% weight concentration aqueous potassium hydroxide solution were charged into a 1-liter flask, and the unneutralized product was gradually added while stirring to obtain a partially neutralized product with a non-volatile content of 40%.
[0083] (Method for producing P-3-1) 186 g of n-octadecyl alcohol was added to a 500 mL four-neck flask, and while stirring, 34 g of tetraphosphorus hexaoxide was gradually added and reacted to obtain an unneutralized product. 409 g of ion-exchanged water and 71 g of a 50% weight concentration aqueous potassium hydroxide solution were charged into a 1-liter flask, and the unneutralized product was gradually added while stirring, obtaining a partially neutralized product with a non-volatile content of 35%. (Method for producing P-3-2) 181 g of n-octadecyl alcohol was added to a 500 mL four-neck flask, and while stirring, 37.9 g of tetraphosphorus hexaoxide was gradually added and reacted to obtain an unneutralized product. 409 g of ion-exchanged water and 72 g of a 50% weight concentration aqueous potassium hydroxide solution were charged into a 1-liter flask, and the unneutralized product was gradually added while stirring, obtaining a partially neutralized product with a non-volatile content of 35%. (Method for producing P-3-3) 153 g of n-octadecyl alcohol was added to a 500 mL four-neck flask, and while stirring, 32.4 g of tetraphosphorus decanoate was gradually added and reacted to obtain an unneutralized product. 468 g of ion-exchanged water, 28.0 g of a 50% weight concentration aqueous potassium hydroxide solution, and 18.6 g of triethanolamine were charged to a 1-liter flask, and the unneutralized product was gradually added while stirring to obtain a partially neutralized product with a nonvolatile content of 30%.
[0084] (Method for producing P-4-1) 166 g of n-docosyl alcohol was added to a 500 mL four-neck flask, and while stirring, 26.5 g of tetraphosphorus hexaoxide was gradually added and reacted to obtain an unneutralized product. 453 g of ion-exchanged water and 55 g of a 50% weight concentration aqueous potassium hydroxide solution were charged to a 1-liter flask, and the unneutralized product was gradually added with stirring to obtain a partially neutralized product with a non-volatile content of 30%. (Method for producing P-4-2) 163 g of n-docosyl alcohol and 7.6 g of 75% phosphoric acid were added to a 500 mL four-neck flask, and while stirring, 24.2 g of tetraphosphorus hexaoxide was gradually added and reacted to obtain an unneutralized product. 446 g of ion-exchanged water and 60 g of a 50% weight concentration aqueous potassium hydroxide solution were charged to a 1-liter flask, and the unneutralized product was gradually added with stirring to obtain a partially neutralized product with a non-volatile content of 30%.
[0085] (Method for producing P-5-1) 182 g of iso-octadecyl alcohol was added to a 500 mL four-neck flask, and while stirring, 35.8 g of tetraphosphorus decanoate was gradually added and reacted to obtain an unneutralized product. 408 g of ion-exchanged water and 74 g of a 50% weight concentration aqueous potassium hydroxide solution were charged to a 1-liter flask, and the unneutralized product was gradually added while stirring to obtain a partially neutralized product with a nonvolatile content of 35%.
[0086] (Production method of p-1) 207 g of 2-ethylhexyl alcohol was added to a 500 mL four-neck flask, and while stirring, 88.8 g of tetraphosphorus decanoate was gradually added to cause a reaction, yielding an unneutralized product. 264 g of ion-exchanged water and 140 g of a 50% weight concentration aqueous potassium hydroxide solution were charged to a 1-liter flask, and the unneutralized product was gradually added while stirring, yielding a partially neutralized product with a nonvolatile content of 50%.
[0087] (Production method of p-2) 220 g of n-dodecyl alcohol was added to a 500 mL four-neck flask, and while stirring, tetraphosphorus decanoate was gradually added to the mixture so that a total amount of 74.1 g was obtained, resulting in a reaction, and an unneutralized product was obtained. 285 g of ion-exchanged water and 121 g of a 50% weight concentration aqueous potassium hydroxide solution were charged to a 1-liter flask, and the unneutralized product was gradually added to the mixture while stirring, resulting in a partially neutralized product with a nonvolatile content of 50%.
[0088] [Nonionic Surfactant (B)] The nonionic surfactants (B) used in the examples and comparative examples are those shown in Table 9 and are as follows: B-6: Polyoxyethylene (10) dodecylamino ether B-7: Polyoxyethylene (5) C12-13 secondary alkyl ether B-8: Polyoxyethylene (20) sorbitan monooleate
[0089] [Preparation of First and Second Treatment Agents] An organic phosphate ester compound, a nonionic surfactant (B), and the following component (C) were mixed to obtain the content ratios in the nonvolatile content shown in Tables 10 and 11, to obtain a first treatment agent and a second treatment agent. (Component (C)) C-1: Mineral oil (viscosity 80 seconds) C-2: Dioctyl sulfosuccinate sodium salt C-3: Sulfated beef tallow sodium salt
[0090] Examples 1-16 and Comparative Examples 1-8: The first and second treatment agents were diluted with 70°C hot water at the ratios shown in Tables 1-3 to obtain diluted solutions with a nonvolatile content of 0.6% by weight. Next, 2,000 g of each diluted solution of the regenerated cellulose fiber treatment agent was applied to 100 g of fiber body using the dip-oiling method at a liquid temperature of 50°C, resulting in a nonvolatile content of 0.20% by weight of the regenerated cellulose fiber treatment agent adhered to the fiber. The fiber body was viscose rayon fiber with a single fiber fineness of 1.3 Dtex and a fiber length of 38 mm, to which no regenerated cellulose fiber treatment agent had been applied. The fibers to which each diluted solution of the regenerated cellulose fiber treatment agent had been applied were placed in a hot air dryer at 105°C for 90 minutes and then left to dry at room temperature for at least 8 hours to obtain cotton treated with the regenerated cellulose fiber treatment agent.
[0091] [Nep suppression] In an atmosphere of 30°C x 65% RH, 40 g of cotton treated with the treatment agent was subjected to an opening treatment using a fiber opening machine (model OP-400) manufactured by Yamato Kiko Co., Ltd. The opened cotton treated with the treatment agent was then fed into a random carding machine, and the discharged fleece was layered to form a nep-preventing fabric with a basis weight of 100 g / m. 2 A fiber web of the above formula was obtained. This fiber web was fed to a drawing frame (Hara Loom Works, Ltd.) and passed three times at a spinning speed of 700 m / min. Five grams of the resulting drawing sliver was taken and the number of neps was measured. Evaluation was made based on the following criteria, with ⊚ and ◯ representing passing. ⊚ (very good): The number of neps per 1 g of drawing sliver was less than 90. ◯ (good): The number of neps per 1 g of drawing sliver was 90 or more but less than 110. △ (poor): The number of neps per 1 g of drawing sliver was 110 or more but less than 130. × (very poor): The number of neps per 1 g of drawing sliver was 130 or more.
[0092] [Fiber bundling] In an atmosphere of 30°C x 65% RH, 40 g of cotton treated with the treatment agent was subjected to an opening treatment using a fiber opening machine (model OP-400) manufactured by Yamato Kiko Co., Ltd. The opened cotton treated with the treatment agent was then fed into a random carding machine, and the discharged fleece was layered to form a fiber bundle with a basis weight of 100 g / m. 2A fiber web of the above formula was obtained. A 10 cm x 5 cm tensile test specimen was prepared from this fiber web and subjected to a tensile test at a speed of 50 m / min. The tensile test was performed using a tension / compression tester (TG-2kN type tension / compression tester, manufactured by Minebea Co., Ltd.) under conditions of a load cell of 50 N in a room at 20°C, and the results were evaluated based on the following evaluation criteria, with ⊚ and ◯ representing pass. ⊚ (very good): pull-out resistance of 2.0 N or more ◯ (good): pull-out resistance of 1.7 N or more but less than 2.0 N △ (poor): pull-out resistance of 1.4 N or more but less than 1.7 N × (very poor): pull-out resistance of less than 1.4 N
[0093] [Yarn Quality of Spun Yarn] 200 g of treated cotton was opened, carded, drawn, and roving-spun on a miniature spinning machine to produce a roving. This roving was spun on a Toyota Industries Corporation ring spinning machine (model RX-240NEW-EST / E) at 30°C and 65% RH to obtain a spun yarn. The resulting spun yarn was measured for U% using an automatic yarn unevenness tester. U% is calculated by selecting a certain measurement length (L) as shown in Figure 1 , defining the area enclosed by the average yarn thickness (X), -100%, the starting point (A), and the end point (B) within that interval as F, and defining the area enclosed by the variation in yarn thickness (unevenness curve) within the interval as f, as follows: U(%) = (f / F) × 100. The yarn quality of the spun yarn was evaluated based on the measured U% using the following evaluation criteria, with ○ representing a pass rating. ◯ (Good): U% is less than 10. × (bad): U% is 10 or more.
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[0105] As can be seen from Tables 1 and 2, the treatment agents for regenerated cellulose fibers in Examples 1 to 16 contain an organic phosphate ester compound (A) and a nonionic surfactant (B), and the weight ratio (A / B) of the compound (A) to the surfactant (B) is 0.05 to 1.0, so that they have good nep suppression properties and produce good yarn quality.
[0106] On the other hand, as can be seen from Table 3, when the organic phosphate ester compound (A) was not contained (Comparative Examples 1 to 3, 7, and 8), when the nonionic surfactant (B) was not contained (Comparative Example 5), and when the organic phosphate ester compound (A) and the nonionic surfactant (B) were contained but the weight ratio (A / B) was not 0.05 to 1.0 (Comparative Examples 4 and 6), the problem of nep suppression, which is an issue of the present application, was not resolved, and the yarn quality was poor.
[0107] Regenerated cellulose fibers treated with the treating agent for regenerated cellulose fibers of the present invention have good nep suppression properties, resulting in high-quality fiber structures, and can be used for spun yarns, nonwoven fabrics, etc.
Claims
1. A treatment agent for regenerated cellulose fibers, comprising the following organic phosphate ester compound (A) and nonionic surfactant (B), wherein the weight ratio (A / B) of compound (A) to surfactant (B) is 0.05 to 1.0: Organic phosphate ester compound (A): An organic phosphate ester compound having a hydrocarbon group having 14 to 22 carbon atoms, including compound (A1) represented by the following general formula (1) and compound (A2) represented by the following general formula (2): (In formula (1), R 1 is a monovalent saturated hydrocarbon group having 14 to 22 carbon atoms. 1 and M 2 are each independently a hydrogen atom, an alkali metal, ammonium, phosphonium, an organic amine, or a quaternary ammonium. (In formula (2), R 2 and R 3 are each independently a monovalent saturated hydrocarbon group having 14 to 22 carbon atoms. 1 is a hydrogen atom, an alkali metal, ammonium, phosphonium, an organic amine, or a quaternary ammonium.
2. The treatment agent for regenerated cellulose fibers according to claim 1, wherein the compound (A) optionally contains a compound (A3) represented by the following general formula (3), and the weight ratio of the compound (A1) to the total of the compounds (A1), (A2), and (A3) (A1 / (A1+A2+A3)) is 0.01 to 0.
6. (In formula (3), R 4 is a monovalent saturated hydrocarbon group having 14 to 22 carbon atoms. 1 and M 2 are each independently a hydrogen atom, an alkali metal, ammonium, phosphonium, an organic amine, or a quaternary ammonium. 2 or R 5 It is. 5 is a monovalent saturated hydrocarbon group having 14 to 22 carbon atoms. Y is 1 or 2. M 2 When there are two or more, they may be the same or different.) 3. The treatment agent for regenerated cellulose fibers according to claim 2, wherein the compound (A) includes a compound (A3) represented by the general formula (3).
4. The compound (A) is 1 is a monovalent saturated hydrocarbon group having 16 to 22 carbon atoms; and 2 and R 3 The treatment agent for regenerated cellulose fibers according to any one of claims 1 to 3, comprising at least one compound selected from the group consisting of compounds represented by general formula (2), each of which is independently a monovalent saturated hydrocarbon group having 16 to 22 carbon atoms.
5. The agent for treating regenerated cellulose fibers according to any one of claims 1 to 4, wherein the acid value of the nonvolatile content of the agent for treating regenerated cellulose fibers is 0.1 to 70 mgKOH / g.
6. A treatment agent for regenerated cellulose fibers according to any one of claims 1 to 5, wherein the nonionic surfactant (B) comprises at least one selected from the group consisting of a compound represented by the following general formula (4) and a nitrogen-containing nonionic surfactant: (In formula (4), R 6 is an alkyl group having 8 to 22 carbon atoms, an alkenyl group having 8 to 22 carbon atoms, an alkanoyl group having 8 to 22 carbon atoms, or an alkenoyl group having 8 to 22 carbon atoms. 7 is a hydrogen atom, an alkyl group having 8 to 22 carbon atoms, an alkenyl group having 8 to 22 carbon atoms, an alkanoyl group having 8 to 22 carbon atoms, or an alkenoyl group having 8 to 22 carbon atoms. a and b are each an integer of 0 to 20, and satisfy the relationship 3≦a+b≦40. 3 H 6 O) and (C 2 H 4 O) may be arranged randomly or in blocks.
7. The regenerated cellulose fiber treating agent according to any one of claims 1 to 6, which is used for spinning regenerated cellulose.
8. A treatment agent for regenerated cellulose fibers described in any one of claims 1 to 7, which is composed of a set of multiple treatment agents including a multi-component first treatment agent for regenerated cellulose fibers containing the compound (A) and a multi-component second treatment agent for regenerated cellulose fibers containing the nonionic surfactant (B).
9. A multi-component first treatment agent for regenerated cellulose fibers used as a treatment agent for regenerated cellulose fibers according to any one of claims 1 to 7, wherein the treatment agent for regenerated cellulose fibers is a treatment agent for regenerated cellulose fibers composed of a set of multiple treatment agents, and the multi-component first treatment agent for regenerated cellulose fibers contains the compound (A) and is used in combination with a multi-component second treatment agent for regenerated cellulose fibers containing the nonionic surfactant (B).
10. A multi-component second treatment agent for regenerated cellulose fibers used as a treatment agent for regenerated cellulose fibers according to any one of claims 1 to 7, wherein the treatment agent for regenerated cellulose fibers is a treatment agent for regenerated cellulose fibers composed of a set of multiple treatment agents, and the multi-component second treatment agent for regenerated cellulose fibers contains the nonionic surfactant (B) and is used in combination with a multi-component first treatment agent for regenerated cellulose fibers containing the compound (A).
11. Regenerated cellulose fibers to which the treatment agent for regenerated cellulose fibers according to any one of claims 1 to 8 has been applied.
12. A spun yarn comprising the regenerated cellulose fibers of claim 11.
Citation Information
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