TW201610262A - Treating agent for synthetic fiber and use thereof - Google Patents
Treating agent for synthetic fiber and use thereof Download PDFInfo
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- TW201610262A TW201610262A TW104122272A TW104122272A TW201610262A TW 201610262 A TW201610262 A TW 201610262A TW 104122272 A TW104122272 A TW 104122272A TW 104122272 A TW104122272 A TW 104122272A TW 201610262 A TW201610262 A TW 201610262A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
- D06M13/256—Sulfonated compounds esters thereof, e.g. sultones
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K15/00—Anti-oxidant compositions; Compositions inhibiting chemical change
- C09K15/04—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds
- C09K15/12—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds containing sulfur and oxygen
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K15/00—Anti-oxidant compositions; Compositions inhibiting chemical change
- C09K15/04—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
- D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
- D06M13/295—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof containing polyglycol moieties; containing neopentyl moieties
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Abstract
Description
本發明關於合成纖維用處理劑及其利用。更詳細來說,有關製造合成纖維樹脂時使用的合成纖維用處理劑、使用該處理劑的合成纖維長絲紗線的製造方法及與包含該合成纖維長絲紗線的纖維結構物。 The present invention relates to a treating agent for synthetic fibers and use thereof. More specifically, the method for producing a synthetic fiber used in the production of a synthetic fiber resin, a method for producing a synthetic fiber filament yarn using the treating agent, and a fiber structure including the synthetic fiber filament yarn.
一直以來,用纖維油劑處理過的纖維被暫時捲曲,並被用在拉伸步驟中,但最近採用縮短該步驟而將上油(oiling)紗直接用在拉伸步驟的方法。 Fibers treated with a fiber oil agent have been temporarily crimped and used in the stretching step, but recently, a method of shortening this step to directly apply an oiling yarn to the stretching step has been employed.
該方法中,在拉伸步驟中,一旦發生斷紗等問題,會導致大量的纖維損失,因此,需要極力避免在拉伸步驟中產生問題。問題的產生的主要原因是紗線斷裂等的纖維損傷,為了防止此問題,需要潤滑性與耐熱性優異的合成纖維用處理劑。 In this method, in the stretching step, if a problem such as yarn breakage occurs, a large amount of fiber loss is caused, and therefore, it is necessary to avoid the occurrence of a problem in the stretching step as much as possible. The cause of the problem is fiber damage such as yarn breakage, and in order to prevent this problem, a treatment agent for synthetic fibers excellent in lubricity and heat resistance is required.
再者,嘗試著纖維的高强力化、低收縮率化之物性提高、生產時的多端化、高速化之生產性的提高,以至今未成為問題的輥污染為原因,產生絨毛、斷紗增加的問題。因此被指出:為了將輥保持為清潔狀態,要使輥的清掃間 隔縮短,清掃次數增加,生產性降低。 In addition, attempts have been made to increase the fiber strength, to improve the physical properties of the low shrinkage rate, to improve the productivity of the end of production, and to improve the productivity of the machine, and to increase the pile and the yarn breakage due to the roll contamination that has not been a problem so far. The problem. Therefore, it is pointed out that in order to keep the roller in a clean state, the cleaning room of the roller is required. The interval is shortened, the number of cleanings is increased, and productivity is lowered.
針對該問題,在專利文獻1中提出有併用磷酸酯系陰離子界面活性劑與磺酸酯系陰離子界面活性劑的合成纖維用處理劑。但是,該處理劑以紡錘(spindle)方式使用時存在如下缺點:耐熱性與潤滑性不充分,熱劣化後的油劑成分等累積於拉伸輥而使摩擦經時上升,拉伸步驟中產生斷紗、纖維品質劣化。 In order to solve this problem, Patent Document 1 proposes a treatment agent for synthetic fibers in which a phosphate ester anionic surfactant and a sulfonate anion surfactant are used in combination. However, when the treating agent is used in the form of a spindle, there are disadvantages in that heat resistance and lubricity are insufficient, and oil component or the like after thermal deterioration is accumulated in the stretching roll to increase the frictional time, and is generated in the stretching step. Broken yarn and deteriorated fiber quality.
此外,專利文獻1中,還提出有在上述陰離子界面活性劑中併用了特定的酯與抗氧化劑的處理劑。但是,即使是如此的處理劑,也無法得到滿足嚴格的制紗條件的耐熱性。 Further, Patent Document 1 proposes a treatment agent in which a specific ester and an antioxidant are used in combination with the above anionic surfactant. However, even with such a treatment agent, heat resistance which satisfies strict yarn making conditions cannot be obtained.
再者,針對上述問題,專利文獻2中提出併用多元醇的酯、具有硫醚基的羧酸與醇的酯、二級磺酸酯、烷基磷酸酯、受阻酚系抗氧化劑而得到的處理劑。但是,對於實現高强力化、低收縮率化、高速化之生產性的提高從而目前為止沒有成為問題的輥污染所導致的絨毛、斷紗,即使使用了該處理劑,也無法得到改善。此外,在使用了專利文獻2中記載的抗氧化劑的情況下,纖維的保管中還存在纖維會漸漸變色的缺點。 Further, in order to solve the above problems, Patent Document 2 proposes a treatment in which an ester of a polyhydric alcohol, an ester of a carboxylic acid having a thioether group and an alcohol, a secondary sulfonate, an alkyl phosphate, or a hindered phenol antioxidant is used. Agent. However, in order to improve the productivity of high-strength, low-shrinkage, and high-speed, there has been no problem of fluff and yarn breakage caused by roll contamination, and even if the treatment agent is used, it cannot be improved. Further, when the antioxidant described in Patent Document 2 is used, there is a disadvantage that the fibers gradually become colored during storage of the fibers.
因此,期望得到能夠抑制由於輥的清掃間隔縮短、清掃次數增加而導致生產性的降低、耐熱性優異的處理劑。 Therefore, it is desired to obtain a treatment agent capable of suppressing a decrease in productivity due to a shortened cleaning interval of the rolls and an increase in the number of cleanings, and excellent heat resistance.
[專利文獻1]日本特開昭59-211680號公報 [Patent Document 1] Japanese Laid-Open Patent Publication No. 59-211680
[專利文獻2]日本特開平8-120563號公報 [Patent Document 2] Japanese Patent Laid-Open No. Hei 8-120563
本發明的目的在於提供一種於製造合成樹脂時使用,能夠降低輥污染且耐熱性優異的合成纖維用處理劑、使用該處理劑的合成纖維長絲紗線的製造方法、以及包含用該製造方法得到的合成纖維長絲紗線的纖維結構物。 An object of the present invention is to provide a treatment agent for synthetic fibers which can be used in the production of a synthetic resin, which can reduce roll contamination and has excellent heat resistance, a method for producing a synthetic fiber filament yarn using the treatment agent, and a method for producing the same. A fiber structure of the obtained synthetic fiber filament yarn.
本發明人們進行了深入研究的結果,首先發現:1)於含有由通式(1)表示的有機磺酸化合物的原料中大量含有硫酸鈉、氯化鈉;2)處理劑中所含有的硫酸鈉或氯化鈉會在紡紗時脫落、累積在拉伸輥上,從而引起斷紗斷線的增加,而且在進行熱拉伸的輥上,加快積存焦油,引起輥污染。因此,3)藉由將從處理劑的不揮發成分中檢測出的硫酸根離子(SO4 2-)及氯離子(Cl-)設為規定的比率以下,能夠急劇降低輥污染,由此至此完成本發明。 As a result of intensive studies, the inventors have found that: 1) a large amount of sodium sulfate and sodium chloride are contained in a raw material containing an organic sulfonic acid compound represented by the general formula (1); 2) sulfuric acid contained in the treating agent Sodium or sodium chloride will fall off during the spinning and accumulate on the stretching rolls, causing an increase in broken yarn breakage, and accelerating the accumulation of tar on the rolls subjected to hot stretching, causing roll contamination. Therefore, 3) by setting the sulfate ion (SO 4 2- ) and the chloride ion (Cl − ) detected from the nonvolatile component of the treatment agent to a predetermined ratio or less, the roll contamination can be drastically reduced, thereby The present invention has been completed.
即,本發明的合成纖維用處理劑係含有平滑成分(A)與由下述通式(1)表示的有機磺酸化合物(B),並且,前述有機磺酸化合物(B)在處理劑的不揮發成分中所佔的重量比率為1.25至12重量%,藉由離子色譜法從處理劑的不揮發成分中檢測出的硫酸根離子(SO4 2-)的重量比率為 200ppm以下,氯離子(Cl-)的重量比率為200ppm以下。 In other words, the treating agent for synthetic fibers of the present invention contains the smoothing component (A) and the organic sulfonic acid compound (B) represented by the following general formula (1), and the organic sulfonic acid compound (B) is in the treating agent. The weight ratio of the non-volatile component is 1.25 to 12% by weight, and the weight ratio of sulfate ion (SO 4 2- ) detected from the nonvolatile matter of the treating agent by ion chromatography is 200 ppm or less, chloride ion The weight ratio of (Cl - ) is 200 ppm or less.
(式(1)中,a及b為0以上的整數且是滿足a+b=5至17的整數。M為氫原子、鹼金屬、銨基或有機胺基)。 (In the formula (1), a and b are integers of 0 or more and are integers satisfying a+b=5 to 17. M is a hydrogen atom, an alkali metal, an ammonium group or an organic amine group).
前述平滑成分(A)在處理劑中所佔的重量比率,較佳為20至70重量%。 The weight ratio of the smoothing component (A) to the treating agent is preferably from 20 to 70% by weight.
前述有機磺酸化合物(B)在處理劑的不揮發成分中所佔的重量比率,較佳為1.25至7重量%。 The weight ratio of the organic sulfonic acid compound (B) to the nonvolatile matter of the treating agent is preferably 1.25 to 7% by weight.
本發明的處理劑更含有有機磷酸酯化合物(C),並且藉由離子色譜法從處理劑的不揮發成分中檢測出的磷酸根離子(PO4 3-)的重量比率為500ppm以下為較佳。 The treatment agent of the present invention further contains the organic phosphate compound (C), and the weight ratio of the phosphate ion (PO 4 3- ) detected from the nonvolatile matter of the treatment agent by ion chromatography is preferably 500 ppm or less. .
前述有機磷酸酯化合物(C)在處理劑的不揮發成分中所佔的重量比率,較佳為0.05至5重量%。 The weight ratio of the above organophosphate compound (C) to the nonvolatile content of the treating agent is preferably from 0.05 to 5% by weight.
前述有機磷酸酯化合物(C)係選自由下述通式(2)表示的化合物及由下述通式(3)表示的化合物之至少一種。 The organophosphate compound (C) is at least one selected from the group consisting of a compound represented by the following formula (2) and a compound represented by the following formula (3).
(式(2)中,R1為碳原子數6至24的烴基。A1O為碳原子數2至4的氧伸烷基(oxyalkylene),m為0至15的整數,n為1至2的整數。M1為氫原子、鹼金屬、銨基或有機胺基)。 (In the formula (2), R 1 is a hydrocarbon group having 6 to 24 carbon atoms. A 1 O is an oxyalkylene having 2 to 4 carbon atoms, m is an integer of 0 to 15, and n is 1 to An integer of 2, M 1 is a hydrogen atom, an alkali metal, an ammonium group or an organic amine group).
(式(3)中,R1為碳原子數6至24的烴基。A1O為碳原子數2至4的氧伸烷基,m為0至15的整數。M1為氫原子、鹼金屬、銨基或有機胺基。Q1為M1或R1O(A1O)m。Y為1或2)。 (In the formula (3), R 1 is a hydrocarbon group having 6 to 24 carbon atoms. A 1 O is an oxygen alkyl group having 2 to 4 carbon atoms, and m is an integer of 0 to 15. M 1 is a hydrogen atom or a base. a metal, ammonium or organic amine group. Q 1 is M 1 or R 1 O(A 1 O) m . Y is 1 or 2).
本發明的處理劑更含有非離子界面活性劑(D)為較佳。 It is preferred that the treating agent of the present invention further contains a nonionic surfactant (D).
前述非離子界面活性劑(D)在處理劑的不揮發成分中所佔的重量比率,較佳為20至70重量%。 The weight ratio of the nonionic surfactant (D) to the nonvolatile component of the treating agent is preferably from 20 to 70% by weight.
本發明的合成纖維長絲紗線係於原料合成纖維長絲紗線賦予上述處理劑而成者。 The synthetic fiber filament yarn of the present invention is obtained by providing the above-mentioned treating agent to the raw material synthetic fiber filament yarn.
本發明的合成纖維長絲紗線的製造方法係 包括於原料合成纖維長絲紗線賦予上述處理劑的步驟。 The method for producing the synthetic fiber filament yarn of the present invention is The step of imparting the above treating agent to the raw material synthetic fiber filament yarn.
本發明的纖維結構物係包含上述合成纖維長絲紗線及/或用上述製造方法得到的合成纖維長絲紗線。 The fiber structure of the present invention comprises the above-mentioned synthetic fiber filament yarn and/or the synthetic fiber filament yarn obtained by the above production method.
使用本發明的合成纖維用處理劑的情況下,能夠降低製造合成纖維時的輥污染,且耐熱性優異。其結果,增長輥的清掃間隔,能夠減少其清掃次數,能實現合成纖維的生產性提高。 When the treating agent for synthetic fibers of the present invention is used, roll contamination at the time of producing synthetic fibers can be reduced, and heat resistance is excellent. As a result, the cleaning interval of the growth rolls can reduce the number of times of cleaning, and the productivity of synthetic fibers can be improved.
根據本發明的製造方法,能降低浮渣或斷紗的產生,能夠得到紗品質優異的合成纖維長絲紗線。本發明的纖維結構物品質優異。 According to the production method of the present invention, it is possible to reduce the occurrence of scum or yarn breakage, and it is possible to obtain a synthetic fiber filament yarn excellent in yarn quality. The fiber structure of the present invention is excellent in quality.
本發明的合成纖維用處理劑含有平滑成分(A)與由上述通式(1)表示的有機磺酸化合物(B),並使利用離子色譜法從處理劑的不揮發成分中檢測出的硫酸根離子與氯離子為規定濃度以下。以下,進行詳細說明。 The treating agent for synthetic fibers of the present invention contains the smoothing component (A) and the organic sulfonic acid compound (B) represented by the above formula (1), and the sulfuric acid detected from the nonvolatile matter of the treating agent by ion chromatography. The root ion and the chloride ion are below a predetermined concentration. The details will be described below.
平滑成分(A)為本發明的處理劑的必需成分。作為平滑成分(A),可以列舉:1)具有脂肪族一元醇與脂肪酸所形成的酯鍵結構的酯化合物(A1)、2)具有脂肪族多元醇與脂肪酸所形成的酯鍵結構的酯化合物(A2)、3)具有脂肪族一元 醇與脂肪族多元羧酸所形成的酯鍵結構的酯化合物(A3)、4)分子內具有芳香環的芳香族酯化合物(A4)、5)含硫的酯化合物(A5)、6)礦物油(A6)等之一般被用作合成纖維處理劑的公知的平滑成分。平滑成分(A)可以使用1種或2種以上。 The smoothing component (A) is an essential component of the treating agent of the present invention. Examples of the smoothing component (A) include: 1) an ester compound having an ester bond structure formed by an aliphatic monohydric alcohol and a fatty acid (A1), and 2) an ester compound having an ester bond structure formed by an aliphatic polyol and a fatty acid. (A2), 3) have an aliphatic one dollar An ester bond structure ester compound (A3) formed by an alcohol and an aliphatic polycarboxylic acid, 4) an aromatic ester compound (A4) having an aromatic ring in the molecule, 5) a sulfur-containing ester compound (A5), 6) mineral Oil (A6) or the like is generally used as a known smoothing component of a synthetic fiber treating agent. One or two or more kinds of the smoothing component (A) can be used.
酯化合物(A1)是具有脂肪族一元醇與脂肪酸(脂肪族一元羧酸)所形成的酯鍵結構的化合物,而且是在分子內不具有聚氧伸烷基的化合物。酯化合物(A1)可以使用1種或2種。 The ester compound (A1) is a compound having an ester bond structure formed between an aliphatic monohydric alcohol and a fatty acid (aliphatic monocarboxylic acid), and is a compound having no polyoxyalkylene group in the molecule. One type or two types of ester compounds (A1) can be used.
作為酯化合物(A1),較佳為由下述通式(4)表示的化合物。 The ester compound (A1) is preferably a compound represented by the following formula (4).
RR 22 -COO-R-COO-R 33 (4) (4)
(式中,R2表示碳原子數4至24的烷基或烯基,R3表示碳原子數6至24的烷基或烯基。) (wherein R 2 represents an alkyl group or an alkenyl group having 4 to 24 carbon atoms, and R 3 represents an alkyl group or an alkenyl group having 6 to 24 carbon atoms.)
R2的碳原子數較佳為6至22,更佳為8至20,進一步更佳為10至18。該碳原子數小於4,則由於油膜變弱,因而有可能造成絨毛增加。另一方面,該碳原子數超過24,則纖維金屬間的摩擦增高,有可能造成絨毛增加。R2可以為烷基或烯基中的任一者,但從耐熱性優異的觀點考慮,較佳為烷基。 The number of carbon atoms of R 2 is preferably from 6 to 22, more preferably from 8 to 20, still more preferably from 10 to 18. When the number of carbon atoms is less than 4, the oil film is weakened, so that the pile may be increased. On the other hand, when the number of carbon atoms exceeds 24, the friction between the fiber metals is increased, and the pile may be increased. R 2 may be either an alkyl group or an alkenyl group, but is preferably an alkyl group from the viewpoint of excellent heat resistance.
R3的碳原子數較佳為6至22,更佳為8至20,進一步更佳為10至18。該碳原子數小於6,則油膜變 弱,因而有可能造成絨毛增加。另一方面,該碳原子數超過24,則纖維金屬間的摩擦增高,有可能造成絨毛增加。R3可以為烷基或烯基中的任一者,但從油膜强度高、不易產生絨毛的觀點考慮,較佳為烯基。 The carbon number of R 3 is preferably from 6 to 22, more preferably from 8 to 20, still more preferably from 10 to 18. When the number of carbon atoms is less than 6, the oil film becomes weak, and thus it is possible to cause an increase in fluff. On the other hand, when the number of carbon atoms exceeds 24, the friction between the fiber metals is increased, and the pile may be increased. R 3 may be either an alkyl group or an alkenyl group, but is preferably an alkenyl group from the viewpoint of high oil film strength and difficulty in generating fluff.
作為酯化合物(A1),沒有特別限定,例如可以舉出:2-癸基四癸醯基順芥子酸酯、2-癸基四癸醯基油酸酯、2-辛基十二烷基硬脂酸酯、棕櫚酸異辛基酯、硬脂酸異辛基酯、棕櫚酸丁基酯、硬脂酸丁基酯、油酸丁基酯、油酸異辛基酯、油酸月桂基酯、硬脂酸異十三烷基酯、硬脂酸十六烷基酯、油酸異硬脂醯基酯、辛酸油基酯、月桂酸油基酯、棕櫚酸油基酯、硬脂酸油基酯、油酸油基酯等。此等之中,較佳為2-癸基四癸醯基油酸酯、2-辛基十二烷基硬脂酸酯、棕櫚酸異辛基酯、硬脂酸異辛基酯、油酸月桂基酯、硬脂酸異十三烷基酯、硬脂酸十六烷基酯、油酸異硬脂醯基酯、油酸油基酯。 The ester compound (A1) is not particularly limited, and examples thereof include 2-mercaptotetradecylsuccinate, 2-mercaptotetradecyl oleate, and 2-octyldodecyl hard. Fatty acid ester, isooctyl palmitate, isooctyl stearate, butyl palmitate, butyl stearate, butyl oleate, isooctyl oleate, lauryl oleate , isotridecyl stearate, cetyl stearate, isostearyl oleate, oleyl octylate, oleyl laurate, oleyl palmitate, stearic acid Base ester, oleic acid oleyl ester, and the like. Among these, 2-mercaptotetradecyl oleate, 2-octyldodecyl stearate, isooctyl palmitate, isooctyl stearate, oleic acid are preferred. Lauryl ester, isotridecyl stearate, cetyl stearate, isostearyl oleate, oleyl oleate.
酯化合物(A1)可以使用通常市售的脂肪酸與脂肪族一元醇,藉由公知的方法合成得到。 The ester compound (A1) can be synthesized by a known method using a commercially available fatty acid and an aliphatic monohydric alcohol.
酯化合物(A2)是具有脂肪族多元醇與脂肪酸(脂肪族一元羧酸)所形成的酯鍵結構的化合物,而且是分子內不具有聚氧伸烷基的化合物。酯化合物(A2)可以使用1種或2種以上。 The ester compound (A2) is a compound having an ester bond structure formed of an aliphatic polyol and a fatty acid (aliphatic monocarboxylic acid), and is a compound having no polyoxyalkylene group in the molecule. The ester compound (A2) may be used alone or in combination of two or more.
構成酯化合物(A2)的脂肪族多元醇只要是 二元以上就沒有特別限定,可以使用1種或2種以上。從油膜强度的觀點考慮,多元醇較佳為三元以上,更佳為三元至四元,進一步更佳為三元。 The aliphatic polyol constituting the ester compound (A2) is only The binary or more is not particularly limited, and one type or two or more types can be used. The polyol is preferably ternary or more, more preferably ternary to quaternary, and still more preferably ternary from the viewpoint of oil film strength.
作為脂肪族多元醇,例如可以舉出:乙二醇、二乙二醇、三乙二醇、丙二醇、二丙二醇、三丙二醇、1,2-丁二醇、1,3-丁二醇、1,4-丁二醇、2-甲基-1,3-丙二醇、1,5-戊二醇、1,6-己二醇、新戊二醇、環己二醇、環己烷二甲醇、甘油、三羥甲基丙烷、新戊四醇、赤蘚醇、二甘油、脫水山梨糖醇(sorbitan)、山梨糖醇、二三羥甲基丙烷、二新戊四醇、三甘油、四甘油、蔗糖等。其中,較佳為甘油、三羥甲基丙烷、新戊四醇、赤蘚醇、二甘油、脫水山梨糖醇、山梨糖醇、二三羥甲基丙烷、二新戊四醇、蔗糖,更佳為甘油、三羥甲基丙烷、新戊四醇、赤蘚醇、二甘油、脫水山梨糖醇,進一步更佳為甘油、三羥甲基丙烷。 Examples of the aliphatic polyhydric alcohol include ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, dipropylene glycol, tripropylene glycol, 1,2-butanediol, and 1,3-butylene glycol. , 4-butanediol, 2-methyl-1,3-propanediol, 1,5-pentanediol, 1,6-hexanediol, neopentyl glycol, cyclohexanediol, cyclohexanedimethanol, Glycerin, trimethylolpropane, neopentyl alcohol, erythritol, diglycerin, sorbitan, sorbitol, ditrimethylolpropane, dipentaerythritol, triglycerin, tetraglycerol , sucrose, etc. Among them, preferred are glycerin, trimethylolpropane, neopentyl alcohol, erythritol, diglycerin, sorbitan, sorbitol, ditrimethylolpropane, dipentaerythritol, sucrose, and more. Preferably, it is glycerin, trimethylolpropane, neopentyl alcohol, erythritol, diglycerin, sorbitan, and further preferably glycerin or trimethylolpropane.
構成酯化合物(A2)的脂肪酸可為飽和或不飽和。不飽和鍵的數量沒有特別限定,但在具有3個以上時,氧化導致劣化進行而使處理劑增黏,進而損及潤滑性,因此較佳為1個或2個。作為脂肪酸的碳原子數,從兼顧油膜强度與潤滑性的觀點考慮,較佳為8至24,更佳為10至20,進一步更佳為12至18。脂肪酸可以使用1種或2種以上,亦可以並用飽和脂肪酸及不飽和脂肪酸。 The fatty acid constituting the ester compound (A2) may be saturated or unsaturated. The number of the unsaturated bonds is not particularly limited. However, when three or more are used, oxidation causes deterioration and the treatment agent is thickened, and the lubricity is impaired. Therefore, it is preferably one or two. The number of carbon atoms of the fatty acid is preferably from 8 to 24, more preferably from 10 to 20, still more preferably from 12 to 18, from the viewpoint of achieving both oil film strength and lubricity. One or two or more kinds of the fatty acids may be used, and saturated fatty acids and unsaturated fatty acids may be used in combination.
作為脂肪酸,可以舉出:丁酸、巴豆酸、戊酸、己酸、庚酸、辛酸、壬酸、癸酸、月桂酸、肉豆蔻酸、肉豆蔻油酸、十五烷酸、棕櫚酸、棕櫚油酸、異鯨蠟 酸、十七烷酸、硬脂酸、異硬脂酸、油酸、反式油酸、異油酸、亞油酸、亞麻酸、結核硬脂酸、花生酸、異二十烷酸、鱈油酸(gadoleic acid)、二十烯酸(eicosenoic acid)、二十二烷酸、異二十二烷酸、順芥子酸、二十四烷酸、異二十四烷酸、神經酸、蠟酸、褐煤酸、蜂花酸等。 Examples of the fatty acid include butyric acid, crotonic acid, valeric acid, caproic acid, heptanoic acid, caprylic acid, capric acid, capric acid, lauric acid, myristic acid, myristic acid, pentadecanoic acid, palmitic acid, Palmitoleic acid Acid, heptadecanoic acid, stearic acid, isostearic acid, oleic acid, trans oleic acid, isooleic acid, linoleic acid, linolenic acid, tuberculous stearic acid, arachidic acid, isoicosanoic acid, hydrazine Gadoleic acid, eicosenoic acid, behenic acid, isodocesic acid, sinapic acid, tetracosanoic acid, isotetradecanoic acid, nervonic acid, wax Acid, montanic acid, bee-acid, etc.
此等之中,較佳為辛酸、壬酸、癸酸、月桂酸、肉豆蔻酸、肉豆蔻油酸、十五烷酸、棕櫚酸、棕櫚油酸、異鯨蠟酸、十七烷酸、硬脂酸、異硬脂酸、油酸、反式油酸、異油酸、亞油酸、亞麻酸、結核硬脂酸、花生酸、異二十烷酸、鱈油酸、二十烯酸、二十二烷酸、異二十二烷酸、順芥子酸、二十四烷酸、異二十四碳酸、神經酸,更佳為癸酸、月桂酸、肉豆蔻酸、肉豆蔻油酸、十五烷酸、棕櫚酸、棕櫚油酸、異鯨蠟酸、十七烷酸、硬脂酸、異硬脂酸、油酸、反式油酸、異油酸、亞油酸、亞麻酸、結核硬脂酸、花生酸、異二十烷酸、鱈油酸、二十烯酸,進一步更佳為月桂酸、肉豆蔻酸、肉豆蔻油酸、十五烷酸、棕櫚酸、棕櫚油酸、異鯨蠟酸、十七烷酸、硬脂酸、異硬脂酸、油酸、反式油酸、異油酸、亞油酸、亞麻酸。 Among these, octanoic acid, citric acid, citric acid, lauric acid, myristic acid, myristic acid, pentadecanoic acid, palmitic acid, palmitoleic acid, isoctanic acid, heptadecanoic acid, Stearic acid, isostearic acid, oleic acid, trans-oleic acid, isooleic acid, linoleic acid, linolenic acid, tuberculous stearic acid, arachidic acid, isoicosanoic acid, oleic acid, eicosenoic acid , behenic acid, iso-docosanoic acid, succinic acid, tetracosanoic acid, iso-tetradecanoic acid, nervonic acid, more preferably citric acid, lauric acid, myristic acid, nutmeg oleic acid , pentadecanoic acid, palmitic acid, palmitoleic acid, isocetic acid, heptadecanoic acid, stearic acid, isostearic acid, oleic acid, trans-oleic acid, isooleic acid, linoleic acid, linolenic acid , tuberculous stearic acid, arachidic acid, isoicosanoic acid, oleic acid, eicosa acid, further preferably lauric acid, myristic acid, myristic acid, pentadecanoic acid, palmitic acid, palm oil Acid, isocetic acid, heptadecanoic acid, stearic acid, isostearic acid, oleic acid, trans oleic acid, isooleic acid, linoleic acid, linolenic acid.
酯化合物(A2)是分子內具有2個以上的酯鍵的化合物,但從制紗性的觀點考慮,較佳為分子內具有3個以上的酯鍵的化合物,更佳為分子內具有3個酯鍵的化合物。 The ester compound (A2) is a compound having two or more ester bonds in the molecule, but from the viewpoint of yarn-making property, a compound having three or more ester bonds in the molecule is preferable, and more preferably three in the molecule. Ester-bonded compound.
酯化合物(A2)的碘價沒有特別限定。 The iodine value of the ester compound (A2) is not particularly limited.
酯化合物(A2)的重量平均分子量較佳為300 至1200,更佳為300至1000,進一步更佳為500至1000。在該重量平均分子量小於300時,存在油膜强度不足、絨毛增加的情況,或熱處理時的發煙增加的情況。另一方面,在該重量平均分子量超過1200時,不只是平滑性不足而使絨毛多發,無法得到高品質的纖維,而且存在製織或編織步驟的品質劣化的情況。此外,本發明的重量平均分子量是利用Tosoh(股)製造的凝膠滲透層析儀裝置HLC-8220GPC,以試樣濃度3mg/cc,注入昭與電工(股)製造的分離柱KF-402HQ、KF-403HQ,藉由由示差折射率檢測器測定的譜峰算出。 The weight average molecular weight of the ester compound (A2) is preferably 300. It is preferably 1200, more preferably 300 to 1000, still more preferably 500 to 1000. When the weight average molecular weight is less than 300, there is a case where the oil film strength is insufficient, the pile is increased, or the smoke at the time of heat treatment is increased. On the other hand, when the weight average molecular weight exceeds 1200, not only the smoothness is insufficient, but also the pile is excessively generated, and high-quality fibers cannot be obtained, and the quality of the weaving or weaving step may be deteriorated. Further, the weight average molecular weight of the present invention is a gel permeation chromatography apparatus HLC-8220GPC manufactured by Tosoh Co., Ltd., and is injected into a separation column KF-402HQ manufactured by Showa Electric Co., Ltd. at a sample concentration of 3 mg/cc. KF-403HQ was calculated by the peak of the spectrum measured by the differential refractive index detector.
作為酯化合物(A2),例如可以舉出:三羥甲基丙烷三辛酸酯、三羥甲基丙烷三癸酸酯、三羥甲基丙烷三月桂酸酯、三羥甲基丙烷三油酸酯、三羥甲基丙烷(月桂酸酯、肉豆蔻酸酯、棕櫚酸酯)、三羥甲基丙烷(月桂酸酯、肉豆蔻酸酯、油酸酯)、三羥甲基丙烷(三棕櫚仁脂肪酸酯)、三羥甲基丙烷(三椰子油脂肪酸酯)、三羥甲基丙烷二辛酸酯、三羥甲基丙烷二癸酸酯、三羥甲基丙烷二月桂酸酯、三羥甲基丙烷二油酸酯、三羥甲基丙烷(月桂酸酯、肉豆蔻酸酯)、三羥甲基丙烷(月桂酸酯、油酸酯)、三羥甲基丙烷(肉豆蔻酸酯、油酸酯)、三羥甲基丙烷(二棕櫚仁脂肪酸酯)、三羥甲基丙烷(二椰子油脂肪酸酯)、椰子油、菜籽油、棕櫚油、甘油三月桂酸酯、甘油三油酸酯、甘油三硬脂酸酯、甘油二油酸酯、甘油單月桂酸酯、二甘油二油酸酯、脫水山梨糖醇三油酸酯、脫水山梨糖醇(月桂酸酯、肉 豆蔻酸酯、油酸酯)、脫水山梨糖醇二月桂酸酯、脫水山梨糖醇單油酸酯、新戊四醇四辛酸酯、新戊四醇四癸酸酯、新戊四醇四月桂酸酯、赤蘚醇四月桂酸酯、新戊四醇(四棕櫚仁脂肪酸酯)、新戊四醇(四椰子油脂肪酸酯)、赤蘚醇三油酸酯、赤蘚醇二棕櫚酸酯、1,6-己二醇二油酸酯等。 Examples of the ester compound (A2) include trimethylolpropane trioctanoate, trimethylolpropane tridecanoate, trimethylolpropane trilaurate, and trimethylolpropane trioleate. Ester, trimethylolpropane (laurate, myristate, palmitate), trimethylolpropane (laurate, myristate, oleate), trimethylolpropane (three palms) Kernel fatty acid ester), trimethylolpropane (tri-cocoyl fatty acid ester), trimethylolpropane dioctanoate, trimethylolpropane didecanoate, trimethylolpropane dilaurate, Trimethylolpropane dioleate, trimethylolpropane (laurate, myristate), trimethylolpropane (laurate, oleate), trimethylolpropane (myristic acid) Ester, oleate), trimethylolpropane (dipalmitate fatty acid ester), trimethylolpropane (di-cocoate fatty acid ester), coconut oil, rapeseed oil, palm oil, glycerol trilaurate , glycerol trioleate, glyceryl tristearate, glycerol dioleate, glycerol monolaurate, diglycerin dioleate, sorbitan trioleate, dehydration Sorbitol (laurate, meat) Myristate, oleate), sorbitan dilaurate, sorbitan monooleate, pentaerythritol tetraoctanoate, pentaerythritol tetradecanoate, neopentyl alcohol Laurate, erythritol tetralaurate, pentaerythritol (tetrapalin fatty acid ester), neopentyl alcohol (tetracoconate fatty acid ester), erythritol trioleate, erythritol II Palmitate, 1,6-hexanediol dioleate, and the like.
酯化合物(A2)可以使用採用通常市售的脂肪酸與脂肪族多元醇,利用公知的方法合成得到的物質。並且,天然的果實、種子或花等天然得到的天然酯,係可直接使用滿足酯化合物(A2)的結構之天然酯,或者根據需要可以使用公知的方法對天然酯進行精製,再或者可以使用藉由公知的方法對精製過的酯利用熔點差進行分離、再精製而得到的酯。此外,也可以使用由2種以上的天然酯(油脂)進行酯交換而得到的酯。 As the ester compound (A2), those obtained by a known method can be used by using a commercially available fatty acid and an aliphatic polyol. Further, a natural ester obtained from a natural fruit, a seed, or a flower may be used as it is, or a natural ester which satisfies the structure of the ester compound (A2) may be used as it is, or a natural ester may be purified by a known method as needed, or may be used. The ester obtained by separating and re-refining the purified ester by a difference in melting point by a known method. Further, an ester obtained by transesterification of two or more kinds of natural esters (greases) may also be used.
3)酯化合物(A3) 3) ester compound (A3)
酯化合物(A3)是具有脂肪族一元醇與脂肪族多元羧酸所形成的酯鍵結構的化合物,而且是分子內不具有聚氧伸烷基的化合物。酯化合物(A3)可以使用1種或2種以上。 The ester compound (A3) is a compound having an ester bond structure formed between an aliphatic monohydric alcohol and an aliphatic polycarboxylic acid, and is a compound having no polyoxyalkylene group in the molecule. The ester compound (A3) may be used alone or in combination of two or more.
構成酯化合物(A3)的脂肪族一元醇,沒有特別限定,可以使用1種或2種以上。脂肪族一元醇可以是飽和的或不飽和者。不飽和鍵的數量沒有特別限定,惟具有2個以上時,氧化導致劣化進行而使處理劑增黏,進而損及潤滑性,因此較佳為一個。脂肪族一元醇的碳原子數,從平滑性與油膜强度的觀點考慮,較佳為8至24,更佳為 14至24,進一步更佳為18至22。脂肪族一元醇可以使用1種或2種以上,亦可以併用飽和脂肪酸一元醇與不飽和脂肪族一元醇。 The aliphatic monohydric alcohol constituting the ester compound (A3) is not particularly limited, and one type or two or more types can be used. Aliphatic monohydric alcohols can be saturated or unsaturated. The number of the unsaturated bonds is not particularly limited. However, when there are two or more, oxidation is caused to cause deterioration and the treatment agent is thickened, and the lubricity is impaired. Therefore, it is preferably one. The number of carbon atoms of the aliphatic monohydric alcohol is preferably from 8 to 24, more preferably from the viewpoint of smoothness and oil film strength. Further from 14 to 24, further preferably from 18 to 22. The aliphatic monohydric alcohol may be used singly or in combination of two or more kinds, and a saturated fatty acid monohydric alcohol and an unsaturated aliphatic monohydric alcohol may be used in combination.
作為脂肪族一元醇,可以舉出:辛醇、異辛醇、月桂醇、肉豆蔻醇、肉豆蔻油醇、鯨蠟醇、異鯨蠟醇、棕櫚油醇、硬脂醇、異硬脂醇、油醇、反式油醇、異油醇、鱈油醇、花生醇、異二十烷醇、二十烯醇(eicosenoyl alcohol)、二十二烷醇、異二十二烷醇、順芥子醇、二十四烷醇、異二十四烷醇、神經醇、蠟醇、褐煤醇、蜂花醇等。其中,較佳為辛醇、異辛醇、月桂醇、肉豆蔻醇、肉豆蔻油醇、鯨蠟醇、異鯨蠟醇、棕櫚油醇、硬脂醇、異硬脂醇、油醇、反式油醇、異油醇、鱈油醇、花生醇、異二十烷醇、二十烯醇、二十二烷醇、異二十二烷醇、順芥子醇、二十四烷醇、異二十四烷醇、神經醇,更佳為肉豆蔻油醇、棕櫚醇、油醇、反油醇、異油醇、二十烯醇、二十二碳醇、順芥子醇、神經醇,進一步更佳為油醇、反式油醇、異油醇、鱈油醇、二十烯醇、順芥子醇。 Examples of the aliphatic monohydric alcohol include octanol, isooctyl alcohol, lauryl alcohol, myristyl alcohol, myristyl alcohol, cetyl alcohol, isocetyl alcohol, palmitol alcohol, stearyl alcohol, and isostearyl alcohol. , oleyl alcohol, trans oleyl alcohol, isooleyl alcohol, eucalyptol, arachidyl alcohol, isostearyl alcohol, eicosenoyl alcohol, behenyl alcohol, iso-docosanol, sucrose Alcohol, tetracosyl alcohol, isotetracosyl alcohol, nerol, wax alcohol, montanol, beemel, and the like. Among them, preferred are octanol, isooctanol, lauryl alcohol, myristyl alcohol, myristyl alcohol, cetyl alcohol, isocetyl alcohol, palmitol alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol, and anti Oleohydrin, isooleyl alcohol, eucalyptol, arachidyl alcohol, isostearyl alcohol, eicosyl alcohol, behenyl alcohol, iso-docosanol, sincanol, tetracosyl alcohol, iso Tetracatanol, nervitol, more preferably myristyl oleyl alcohol, palmitol, oleyl alcohol, oleyl alcohol, isooleyl alcohol, eicosyl alcohol, docosa alcohol, sinapyl alcohol, neurool, further More preferred are oleyl alcohol, trans oleyl alcohol, isooleyl alcohol, eucalyptol, eicosyl alcohol, and sinapyl alcohol.
構成酯(A3)的脂肪族多元羧酸只要是二元以上就沒有特別限定,可以使用1種或2種以上。本發明中使用的脂肪族多元羧酸不包括硫代二丙酸等的含硫多元羧酸。脂肪族多元羧酸的價數較佳為二元。同樣,較佳為在分子內不含羥基者。 The aliphatic polyvalent carboxylic acid constituting the ester (A3) is not particularly limited as long as it is two or more, and one type or two or more types can be used. The aliphatic polycarboxylic acid used in the present invention does not include a sulfur-containing polycarboxylic acid such as thiodipropionic acid. The valence of the aliphatic polycarboxylic acid is preferably binary. Also, it is preferred that the hydroxyl group is not contained in the molecule.
作為脂肪族多元羧酸,可以舉出:檸檬酸、異檸檬酸、蘋果酸、烏頭酸、草醯乙酸、草醯琥珀酸、琥 珀酸、延胡索酸、馬來酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸等。其中,較佳烏頭酸、草醯乙酸、草醯琥珀酸、琥珀酸、延胡索酸、馬來酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸,更佳為延胡索酸、馬來酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸。 Examples of the aliphatic polybasic carboxylic acid include citric acid, isocitric acid, malic acid, aconitic acid, oxalic acid, oxalic acid, and succinic acid. Peric acid, fumaric acid, maleic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, and the like. Among them, preferred aconitic acid, oxalic acid, oxalic acid, succinic acid, fumaric acid, maleic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, azelaic acid, Good is fumaric acid, maleic acid, adipic acid, pimelic acid, suberic acid, azelaic acid, azelaic acid.
作為酯化合物(A3),例如可以列舉:己二酸二辛脂、己二酸二月桂酯、己二酸二油酯、己二酸二異鯨蠟酯、癸二酸二辛脂、癸二酸二月桂酯、癸二酸二油酯、癸二酸二異鯨蠟酯等。 Examples of the ester compound (A3) include dioctyl adipate, dilauryl adipate, dioleyl adipate, diiso-cepyl adipate, dioctyl sebacate, and bismuth. Dilauryl acid ester, dioleic acid sebacate, diiso-cetyl sebacate, and the like.
酯化合物(A3)是在分子內具有2個以上的酯鍵的化合物。酯化合物(A3)的碘價沒有特別限定。 The ester compound (A3) is a compound having two or more ester bonds in the molecule. The iodine value of the ester compound (A3) is not particularly limited.
酯化合物(A3)的重量平均分子量較佳為500至1000,更佳為500至800,進一步更佳為500至700。該重量平均分子量小於500時,會有油膜强度不足、絨毛增加,或熱處理時的發煙增加的情況。另一方面,該重量平均分子量超過1000時,熔點增高,成為製織或編織步驟中的浮渣產生的原因,存在品質劣化的情況。 The weight average molecular weight of the ester compound (A3) is preferably from 500 to 1,000, more preferably from 500 to 800, still more preferably from 500 to 700. When the weight average molecular weight is less than 500, there is a case where the oil film strength is insufficient, the pile is increased, or the smoke at the time of heat treatment is increased. On the other hand, when the weight average molecular weight exceeds 1,000, the melting point is increased to cause scum generation in the weaving or weaving step, and the quality may be deteriorated.
酯化合物(A3)可使用通常市售的脂肪族一元醇與脂肪族多元羧酸,採用公知的方法合成而得到。 The ester compound (A3) can be obtained by a known method using a commercially available aliphatic monohydric alcohol and an aliphatic polycarboxylic acid.
芳香族酯化合物(A4)是在分子內至少具有1個芳香環的酯化合物。詳細來說,可以列舉:具有芳香族羧酸與醇所形成的酯鍵結構的酯化合物(A4-1)、具有芳香族醇與羧 酸所形成的酯鍵結構的酯化合物(A4-2)。此外,芳香族酯化合物(A4)是在分子內不具有聚氧伸烷基的化合物。芳香族酯化合物(A4)可以使用1種或2種以上。 The aromatic ester compound (A4) is an ester compound having at least one aromatic ring in the molecule. Specifically, an ester compound (A4-1) having an ester bond structure formed of an aromatic carboxylic acid and an alcohol, and an aromatic alcohol and a carboxy group are mentioned. An ester compound (A4-2) having an ester bond structure formed by an acid. Further, the aromatic ester compound (A4) is a compound which does not have a polyoxyalkylene group in the molecule. One type or two or more types of the aromatic ester compound (A4) can be used.
構成酯化合物(A4-1)的芳香族羧酸可為一元羧酸或多元羧酸。亦可以使用1種或2種以上。 The aromatic carboxylic acid constituting the ester compound (A4-1) may be a monocarboxylic acid or a polycarboxylic acid. One type or two or more types can also be used.
作為芳香族羧酸,可以舉出:苯甲酸、甲苯甲酸、萘甲酸、鄰苯二甲酸、間苯二甲酸、對苯二甲酸、水楊酸、沒食子酸、苯六甲酸、肉桂酸、偏苯三甲酸、均苯四甲酸等。其中,較佳為偏苯三甲酸、鄰苯二甲酸、間苯二甲酸、對苯二甲酸,更佳為偏苯三甲酸。 Examples of the aromatic carboxylic acid include benzoic acid, toluic acid, naphthoic acid, phthalic acid, isophthalic acid, terephthalic acid, salicylic acid, gallic acid, mellitic acid, and cinnamic acid. Trimellitic acid, pyromellitic acid, and the like. Among them, trimellitic acid, phthalic acid, isophthalic acid, and terephthalic acid are preferred, and trimellitic acid is more preferred.
構成酯化合物(A4-1)的醇可為一元醇或多元醇。此外,亦可為脂肪族醇、脂環族醇、芳香族醇中的任一者。一元醇可以使用1種或2種以上。其中,較佳為一元醇,更佳脂肪族一元醇。 The alcohol constituting the ester compound (A4-1) may be a monohydric alcohol or a polyhydric alcohol. Further, it may be any of an aliphatic alcohol, an alicyclic alcohol, and an aromatic alcohol. One type or two or more types may be used for the monohydric alcohol. Among them, a monohydric alcohol is preferred, and an aliphatic monohydric alcohol is preferred.
作為一元醇可以舉出:烷基苯醇、二烷基苯醇、辛醇、異辛醇、月桂醇、肉豆蔻醇、肉豆蔻油醇、鯨蠟醇、異鯨蠟醇、棕櫚油醇、硬脂醇、異硬脂醇、油醇、反油醇、異油醇、鱈油醇、花生醇、異二十烷醇、二十烯醇、二十二烷醇、異二十二烷醇、順芥子醇、二十四烷醇、異二十四烷醇、神經醇、蠟醇、褐煤醇、蜂花醇等。 Examples of the monohydric alcohol include alkyl benzene alcohol, dialkyl benzyl alcohol, octanol, isooctanol, lauryl alcohol, myristyl alcohol, myristyl alcohol, cetyl alcohol, isocetyl alcohol, palmitol alcohol, Stearyl alcohol, isostearyl alcohol, oleyl alcohol, oleyl alcohol, isooleyl alcohol, eucalyptol, arachidyl alcohol, isostearyl alcohol, eicosyl alcohol, behenyl alcohol, iso-docosanol , sinapyl alcohol, tetracosyl alcohol, iso-tetracosyl alcohol, nerol, wax alcohol, montanol, bee algaol, and the like.
作為多元醇,可以列舉:在酯化合物(A2)中說明的脂肪族多元醇、在酯化合物(A4-2)中說明的芳香族多元醇等。 The polyhydric alcohol may, for example, be an aliphatic polyhydric alcohol described in the ester compound (A2) or an aromatic polyhydric alcohol described in the ester compound (A4-2).
構成酯化合物(A4-2)的芳香族醇可以使用1種或2種以上。作為芳香族系醇,較佳為芳香族多元醇, 更佳為芳香族三元醇。 The aromatic alcohol constituting the ester compound (A4-2) may be used alone or in combination of two or more. As the aromatic alcohol, an aromatic polyol is preferred. More preferably, it is an aromatic triol.
作為芳香族醇,可以列舉:烷基苯醇等芳香族一元醇;二烷基苯醇、雙酚A、雙酚Z、1,3,5-三羥基甲基苯等芳香族多元醇等。其中,較佳為雙酚A、雙酚Z、1,3,5-三羥基甲基苯,更佳為1,3,5-三羥基甲基苯。 Examples of the aromatic alcohol include aromatic monohydric alcohols such as alkyl phenyl alcohol; aromatic polyhydric alcohols such as dialkyl phenyl alcohol, bisphenol A, bisphenol Z, and 1,3,5-trihydroxymethylbenzene. Among them, preferred is bisphenol A, bisphenol Z, 1,3,5-trihydroxymethylbenzene, and more preferably 1,3,5-trihydroxymethylbenzene.
構成酯化合物(A4-2)的羧酸可以是脂肪族羧酸、芳香族羧酸中的任一者。此外,亦可為一元羧酸、多元羧酸中的任一者。可以使用1種或2種以上。其中,較佳為一元羧酸,更佳為脂肪酸。從殘留性的觀點考慮,脂肪酸較佳為飽和者。脂肪酸可為直鏈狀或具有支鏈者。 The carboxylic acid constituting the ester compound (A4-2) may be any of an aliphatic carboxylic acid and an aromatic carboxylic acid. Further, it may be any of a monocarboxylic acid and a polyvalent carboxylic acid. One type or two or more types can be used. Among them, a monocarboxylic acid is preferred, and a fatty acid is more preferred. From the standpoint of residual properties, the fatty acid is preferably saturated. The fatty acid may be linear or branched.
作為一元羧酸,可以舉出:烷基苯羧酸、二烷基苯羧酸、丁酸、巴豆酸、戊酸、己酸、庚酸、辛酸、壬酸、癸酸、月桂酸、肉豆蔻酸、肉豆蔻油酸、十五烷酸、棕櫚酸、棕櫚油酸、異鯨蠟酸、十七烷酸、硬脂酸、異硬脂酸、油酸、反式油酸、異油酸、亞油酸、亞麻酸、結核硬脂酸、花生酸、異二十烷酸、鱈油酸、二十烯酸、二十二烷酸、異二十二烷酸、順芥子酸、二十四烷酸、異二十四烷酸、神經酸、蠟酸、褐煤酸、蜂花酸等。 Examples of the monocarboxylic acid include alkylbenzenecarboxylic acid, dialkylbenzenecarboxylic acid, butyric acid, crotonic acid, valeric acid, caproic acid, heptanoic acid, caprylic acid, capric acid, capric acid, lauric acid, and nutmeg. Acid, myristic acid, pentadecanoic acid, palmitic acid, palmitoleic acid, isoctanic acid, heptadecanoic acid, stearic acid, isostearic acid, oleic acid, trans-oleic acid, isooleic acid, Linoleic acid, linolenic acid, tuberculous stearic acid, arachidic acid, isoicosanoic acid, oleic acid, eicosenoic acid, behenic acid, isodocosalic acid, sucrose, twenty-four Alkanoic acid, isotetracosanoic acid, nervonic acid, waxic acid, montanic acid, bee-acid, and the like.
作為多元羧酸,可以舉出:在酯化合物(A3)中說明的脂肪族多元羧酸、在酯化合物(A4-1)中說明的芳香族多元羧酸等。 The polyvalent carboxylic acid may, for example, be an aliphatic polycarboxylic acid described in the ester compound (A3) or an aromatic polycarboxylic acid described in the ester compound (A4-1).
含硫的酯化合物係選自硫代二丙酸與脂肪族醇的二 酯化合物、以及硫代二丙酸與脂肪族醇的單酯化合物中之至少一種。 The sulfur-containing ester compound is selected from the group consisting of thiodipropionic acid and an aliphatic alcohol. An ester compound, and at least one of a monoester compound of thiodipropionic acid and an aliphatic alcohol.
含硫的酯化合物是具有抗氧化能力的成分。藉由使用該含硫的酯化合物,能夠提高處理劑的耐熱性。含硫的酯化合物可以使用1種或2種以上。構成該含硫的酯化合物的硫代二丙酸的分子量較佳為400至1000,更佳為500至900,進一步更佳為600至800。構成該含硫的酯化合物的脂肪族醇可以是飽和或不飽和者。此外,脂肪族醇可為直鏈狀或具有支鏈結構者,但較佳為具有支鏈結構者。脂肪族醇的碳原子數較佳為8至24,更佳為12至24,進一步更佳為16至24。作為脂肪族醇,例如可以舉出:辛醇、2-乙基己基醇、癸醇、月桂醇、肉豆蔻醇、異鯨蠟醇、油醇及異硬脂醇等,其中,較佳為油醇、異硬脂醇。 The sulfur-containing ester compound is a component having an antioxidant ability. By using the sulfur-containing ester compound, the heat resistance of the treatment agent can be improved. The sulfur-containing ester compound may be used alone or in combination of two or more. The molecular weight of the thiodipropionic acid constituting the sulfur-containing ester compound is preferably from 400 to 1,000, more preferably from 500 to 900, still more preferably from 600 to 800. The aliphatic alcohol constituting the sulfur-containing ester compound may be saturated or unsaturated. Further, the aliphatic alcohol may be a linear or branched structure, but preferably has a branched structure. The aliphatic alcohol preferably has 8 to 24 carbon atoms, more preferably 12 to 24 carbon atoms, still more preferably 16 to 24 carbon atoms. Examples of the aliphatic alcohol include octanol, 2-ethylhexyl alcohol, decyl alcohol, lauryl alcohol, myristyl alcohol, isocetyl alcohol, oleyl alcohol, and isostearyl alcohol. Among them, oil is preferred. Alcohol, isostearyl alcohol.
含硫的酯化合物可以為硫代二丙酸與脂肪族醇的二酯化合物(本段落中,簡稱為二酯)、與硫代二丙酸與脂肪族醇的單酯化合物(本段落中,簡稱為單酯)的混合物。此時,二酯與單酯的莫耳比較佳為100/0至70/30,更佳為100/0至75/25,進一步更佳為100/0至80/20。 The sulfur-containing ester compound may be a diester compound of thiodipropionic acid and an aliphatic alcohol (referred to as a diester in this paragraph), a monoester compound with thiodipropionic acid and an aliphatic alcohol (in this paragraph, A mixture of monoesters for short. At this time, the molar ratio of the diester to the monoester is preferably from 100/0 to 70/30, more preferably from 100/0 to 75/25, still more preferably from 100/0 to 80/20.
此外,本發明的合成纖維用處理劑中,作為上述以外的平滑成分,還可以含有礦物油。此處所稱的礦物油不是用來稀釋處理劑的低黏度稀釋劑,而是包含在不揮發成分中。作為礦物油,沒有特別限定,可以舉出:機油、錠子 油、液體石蠟等。礦物油可以使用1種或2種以上。礦物油在30℃下的黏度較佳為100至500秒。 Further, in the treatment agent for synthetic fibers of the present invention, mineral oil may be contained as a smoothing component other than the above. The mineral oil referred to herein is not a low viscosity diluent used to dilute the treatment agent, but is contained in a non-volatile component. The mineral oil is not particularly limited, and examples thereof include motor oil and spindle. Oil, liquid paraffin, etc. One or two or more kinds of mineral oils can be used. The viscosity of the mineral oil at 30 ° C is preferably from 100 to 500 seconds.
作為平滑成分(A),從提高耐熱性的觀點考慮,較佳係使用除去催化劑等並精製過者。 The smoothing component (A) is preferably purified by removing a catalyst or the like from the viewpoint of improving heat resistance.
由上述通式(1)表示的有機磺酸化合物(B)是本發明的處理劑的必要成分。藉由含有平滑成分(A)與有機磺酸化合物(B),並且使藉由離子色譜法從處理劑的不揮發成分中檢測出的硫酸根離子(SO4 2-)的重量比率為200ppm以下、氯離子(Cl-)的重量比率為200ppm以下,從而能夠急劇減少絨毛、斷紗、輥污染。需要說明的是,將硫酸根離子(SO4 2-)簡稱為硫酸根離子,氯離子(Cl-)簡稱為氯離子。 The organic sulfonic acid compound (B) represented by the above formula (1) is an essential component of the treating agent of the present invention. By containing the smoothing component (A) and the organic sulfonic acid compound (B), the weight ratio of sulfate ion (SO 4 2- ) detected from the nonvolatile matter of the treating agent by ion chromatography is 200 ppm or less The weight ratio of chlorine ions (Cl - ) is 200 ppm or less, so that fluff, yarn breakage, and roll contamination can be drastically reduced. It should be noted that the sulfate ion (SO 4 2- ) is simply referred to as a sulfate ion, and the chloride ion (Cl − ) is simply referred to as a chloride ion.
通式(1)中,a與b是0以上的整數且是滿足a+b=5至17的整數。在a+b小於5時,則減少輥污染的效果變小。另一方面,在a+b超過17時,熔點高,處理劑中的相容性變差,而無法使用。a+b較佳為7至17,更佳為10至15。 In the formula (1), a and b are integers of 0 or more and are integers satisfying a+b=5 to 17. When a+b is less than 5, the effect of reducing roll contamination becomes small. On the other hand, when a+b exceeds 17, the melting point is high, and the compatibility in the treating agent is deteriorated, so that it cannot be used. a+b is preferably from 7 to 17, more preferably from 10 to 15.
M為氫原子、鹼金屬、銨基或有機胺基。作為鹼金屬,例如可以列舉:鋰、鈉、鉀等。作為銨基與有機胺基,可以列舉:由NRaRbRcRd表示的基。Ra、Rb、Rc、Rd分別獨立且為氫原子、烷基、烯基、聚氧伸烷基。烷基與烯基的碳原子數較佳為1至24,更佳為1至20,進一步更佳為1至18。聚氧伸烷基以[-(A1O)mH]表示,(A1O)m與由通式(2)表示者相同。 M is a hydrogen atom, an alkali metal, an ammonium group or an organic amine group. Examples of the alkali metal include lithium, sodium, potassium, and the like. Examples of the ammonium group and the organic amine group include a group represented by NR a R b R c R d . R a , R b , R c and R d are each independently a hydrogen atom, an alkyl group, an alkenyl group or a polyoxyalkylene group. The number of carbon atoms of the alkyl group and the alkenyl group is preferably from 1 to 24, more preferably from 1 to 20, still more preferably from 1 to 18. The polyoxyalkylene group is represented by [-(A 1 O) m H], and (A 1 O) m is the same as those represented by the general formula (2).
作為由NRaRbRcRd表示的基,例如可以舉出:銨基、甲基銨基、乙基銨基、丙基銨基、丁基銨基、己基銨基、辛基銨基、二甲基銨基、二乙基銨基、二丙基銨基、二丁基銨基、二己基銨基、二辛基銨基、三甲基銨基、三乙基銨基、三丙基銨基、三丁基銨基、三己基銨基、三辛基銨基、四甲基銨基、四乙基銨基、四丙基銨基、四丁基銨基、四己基銨基、四辛基銨基、乙基三甲基銨基、丙基三甲基銨基、丁基三甲基銨基、己基三甲基銨基、辛基三甲基銨基、甲醇銨基、乙醇銨基、丙醇銨基、丁醇銨基、己醇銨基、辛醇銨基、二甲醇銨基、二乙醇銨基、二丙醇銨基、二丁醇銨基、二己醇銨基、二辛醇銨基、三甲醇銨基、三乙醇銨基、三丙醇銨基、三丁醇銨基、三己醇銨基、三辛醇銨基、(EO6)丁基胺基醚基、(EO6)己基胺基醚基、(EO6)辛基胺基醚基、(EO6)癸基胺基醚基、(EO6)月桂基胺基醚基、(EO6)十四烷基胺基醚基、(EO6)十六烷基胺基醚基、(EO6)油基胺基醚基、(EO6)硬脂基胺基醚基、(EO6)鱈油基胺基醚基、(EO6)二十四烷基胺基醚基、(EO10)油基胺基醚基、(EO10)油基胺基醚基/順芥子酸鹽、(EO3)月桂基胺基醚基、(EO3)月桂基胺基醚基、(EO7)月桂基胺基醚基、(EO15)油基胺基醚基、(PO3、EO5)硬脂基胺基醚基、(PO5、EO3)硬脂基胺基醚基。 Examples of the group represented by NR a R b R c R d include an ammonium group, a methyl ammonium group, an ethyl ammonium group, a propyl ammonium group, a butyl ammonium group, a hexyl ammonium group, and an octyl ammonium group. , dimethyl ammonium, diethyl ammonium, dipropyl ammonium, dibutyl ammonium, dihexyl ammonium, dioctyl ammonium, trimethyl ammonium, triethyl ammonium, tripropyl Alkyl ammonium group, tributyl ammonium group, trihexyl ammonium group, trioctyl ammonium group, tetramethyl ammonium group, tetraethyl ammonium group, tetrapropyl ammonium group, tetrabutyl ammonium group, tetrahexylammonium group, Tetraoctyl ammonium, ethyl trimethyl ammonium, propyl trimethyl ammonium, butyl trimethyl ammonium, hexyl trimethyl ammonium, octyl trimethyl ammonium, ammonium methoxide, ethanol Ammonium, ammonium alkoxide, ammonium butoxide, ammonium hexanoate, ammonium octylate, ammonium dimethoxide, ammonium diethanolate, ammonium dipropoxide, ammonium dibutoxide, ammonium dihexolate , Dioctanol ammonium, trimethylammonium, triethanolammonium, tripropionyl ammonium, tributylammonium, trihexyl ammonium, trioctanol ammonium, (EO6) butylamino ether , (EO6) hexylaminoether group, (EO6) octylamino ether group, (EO6) fluorenyl group Ether group, (EO6) lauryl amine ether group, (EO6) tetradecylamino ether group, (EO6) hexadecylamino ether group, (EO6) oleyl amino ether group, (EO6 ) stearyl amino ether group, (EO6) decyl oleyl ether group, (EO6) tetracosylamino ether group, (EO10) oleyl amino ether group, (EO10) oleyl amine group Ether/succinic acid salt, (EO3) lauryl amine ether group, (EO3) lauryl amine ether group, (EO7) lauryl amine ether group, (EO15) oleyl amino ether group, (PO3 EO5) stearyl amino ether group, (PO5, EO3) stearyl amino ether group.
在包含有機磺酸化合物(B)的原料(以下,稱為原料X)中,其製造方法導致原料含有硫酸鈉及/或氯化鈉。該原料X所包含的硫酸鈉、氯化鈉的比率可以利用離 子色譜法,根據原料X中檢測出的硫酸根離子、氯離子的重量比率來計算。 In the raw material containing the organic sulfonic acid compound (B) (hereinafter referred to as the raw material X), the production method results in the raw material containing sodium sulfate and/or sodium chloride. The ratio of sodium sulfate and sodium chloride contained in the raw material X can be utilized The sub-chromatography is calculated based on the weight ratio of sulfate ion and chloride ion detected in the raw material X.
在原料X含有硫酸鈉的情況下,從原料X中檢測出的硫酸根離子的重量比率相對於有機磺酸化合物(B)為20000ppm以上。此外,在原料X含有氯化鈉的情況下,從原料X中檢測出的氯離子的重量比率相對於有機磺酸化合物(B)為20000ppm以上。 When the raw material X contains sodium sulfate, the weight ratio of the sulfate ion detected from the raw material X is 20,000 ppm or more based on the organic sulfonic acid compound (B). In addition, when the raw material X contains sodium chloride, the weight ratio of the chloride ion detected from the raw material X is 20,000 ppm or more with respect to the organic sulfonic acid compound (B).
在將如此的原料X用在處理劑時,如前所述,硫酸鈉、氯化鈉在紡紗時會脫落並積存在拉伸輥上,引起斷紗斷線的增加。此外,在進行熱拉伸的輥上,硫酸鈉、氯化鈉會加快累積焦油,引起輥污染。作為如此的原料X,可以列舉:HOSTAPUR SAS(Hoechst公司製造)、Mersolat H(拜耳公司製造)等。 When such a raw material X is used as a treating agent, as described above, sodium sulfate and sodium chloride may fall off during spinning and accumulate on the stretching rolls, causing an increase in yarn breakage. In addition, on the rolls subjected to hot stretching, sodium sulfate and sodium chloride accelerate the accumulation of tar, causing roll contamination. Examples of such a raw material X include HOSTAPUR SAS (manufactured by Hoechst Co., Ltd.) and Mersolat H (manufactured by Bayer).
從發揮本發明的效果的觀點考慮,對於本發明的處理劑,使用含有降低來自原料X中的硫酸鈉、氯化鈉的有機磺酸化合物(B)的原料(以下,稱為原料Y)是重要的。具體而言,較佳係藉由離子色譜法從原料Y中檢測出的硫酸根離子的重量比率相對於有機磺酸化合物(B)為5000ppm以下,以及氯離子的重量比率相對於有機磺酸化合物(B)為5000ppm以下。 From the viewpoint of exerting the effects of the present invention, a raw material (hereinafter referred to as a raw material Y) containing an organic sulfonic acid compound (B) which lowers sodium sulfate or sodium chloride derived from the raw material X is used for the treatment agent of the present invention. important. Specifically, it is preferred that the weight ratio of the sulfate ion detected from the raw material Y by ion chromatography is 5000 ppm or less with respect to the organic sulfonic acid compound (B), and the weight ratio of the chloride ion to the organic sulfonic acid compound. (B) is 5,000 ppm or less.
從更加發揮本申請的效果的觀點考慮,相對於有機磺酸化合物(B),從原料Y中檢測出的該硫酸根離子的重量比率更佳為4000ppm以下,進一步更佳為3000ppm以下,特佳為2000ppm以下。同樣,相對於有機磺酸化合物(B),從 原料Y中檢測出的氯離子的重量比率更佳為4000ppm以下,進一步更佳為3000ppm以下,特佳為2000ppm以下。 From the viewpoint of further exerting the effects of the present application, the weight ratio of the sulfate ion detected from the raw material Y to the organic sulfonic acid compound (B) is more preferably 4,000 ppm or less, still more preferably 3,000 ppm or less. It is 2000 ppm or less. Similarly, relative to the organic sulfonic acid compound (B), The weight ratio of the chlorine ions detected in the raw material Y is more preferably 4,000 ppm or less, still more preferably 3,000 ppm or less, and particularly preferably 2,000 ppm or less.
此外,本發明中的藉由離子色譜法進行的硫酸根離子、氯離子的分析方法,係按照實施例中記載的方法。 Further, the method for analyzing sulfate ions and chloride ions by ion chromatography in the present invention is in accordance with the method described in the examples.
作為從含有有機磺酸化合物(B)的原料X中降低硫酸鈉或氯化鈉的方法,沒有特別限定,能夠採用公知的方法。例如可以列舉:在原料X包含硫酸鈉的情況下,在原料X中添加甲醇、水等溶劑,並使硫酸鈉等無機物沉澱析出、分離的方法等。此外,在原料X包含氯化鈉的情況下,可以舉出:藉由離子交換膜除去原料X所包含的氯化鈉的方法、藉由離子交換樹脂進行吸附原料X所包含的氯化鈉的方法等。 The method of reducing sodium sulfate or sodium chloride from the raw material X containing the organic sulfonic acid compound (B) is not particularly limited, and a known method can be employed. For example, when the raw material X contains sodium sulfate, a solvent such as methanol or water is added to the raw material X, and an inorganic substance such as sodium sulfate is precipitated and separated. Further, when the raw material X contains sodium chloride, a method of removing sodium chloride contained in the raw material X by an ion exchange membrane, and adsorbing sodium chloride contained in the raw material X by an ion exchange resin may be mentioned. Method, etc.
上述有機磺酸化合物(B)是具有一個磺酸基的單磺酸化合物。本發明的處理劑除了該單磺酸化合物,亦可以含有由下述通式(5)表示的二磺酸化合物。 The above organic sulfonic acid compound (B) is a monosulfonic acid compound having one sulfonic acid group. The treatment agent of the present invention may contain a disulfonic acid compound represented by the following formula (5) in addition to the monosulfonic acid compound.
式(5)中,c、d與e為0以上的整數,並且是滿足c+d+e=4至16的整數。在c+d+e小於4時,有時降低輥污染的效果變小。另一方面,在c+d+e超過17時,處理劑中的相容性變差,有時無法使用。c+d+e較佳為6至16,更佳為9至14。 In the formula (5), c, d and e are integers of 0 or more, and are integers satisfying c + d + e = 4 to 16. When c+d+e is less than 4, the effect of reducing roll contamination sometimes becomes small. On the other hand, when c+d+e exceeds 17, the compatibility in the treatment agent is deteriorated, and it may not be used. c+d+e is preferably from 6 to 16, more preferably from 9 to 14.
M為氫原子、鹼金屬、銨基或有機胺基。M的說明況與在通式(1)處說明的M相同。 M is a hydrogen atom, an alkali metal, an ammonium group or an organic amine group. The description of M is the same as M described in the general formula (1).
在含有上述二磺酸化合物的情況下,屬於有機磺酸化合物(B)的單磺酸化合物與由通式(5)表示的二磺酸化合物的重量比率(單磺酸化合物/二磺酸化合物)較佳為50/50至99/1,更佳為70/30至99/1,進一步更佳為80/20至98/2。 In the case of containing the above disulfonic acid compound, the weight ratio of the monosulfonic acid compound belonging to the organic sulfonic acid compound (B) to the disulfonic acid compound represented by the general formula (5) (monosulfonic acid compound / disulfonic acid compound) It is preferably 50/50 to 99/1, more preferably 70/30 to 99/1, still more preferably 80/20 to 98/2.
本發明的處理劑中,從減少絨毛的觀點考慮,除了上述平滑成分(A)、有機磺酸化合物(B),較佳係更含有有機磷酸酯化合物(C)。作為有機磷酸酯化合物(C),較佳係選自由上述通式(2)表示的化合物及由上述通式(3)表示的化合物之至少一種。 In the treatment agent of the present invention, in addition to the smoothing component (A) and the organic sulfonic acid compound (B), it is preferred to further contain the organic phosphate compound (C) from the viewpoint of reducing the pile. The organic phosphate compound (C) is preferably at least one selected from the group consisting of the compound represented by the above formula (2) and the compound represented by the above formula (3).
通式(2)及(3)中,R1為碳原子數6至24的烴基。A1O為碳原子數2至4的氧伸烷基,m為0至15的整數。n為1至2的整數。M1為氫原子、鹼金屬、銨基或有機胺基。Q1為M1或R1O(A1O)m。Y為1或2。 In the general formulae (2) and (3), R 1 is a hydrocarbon group having 6 to 24 carbon atoms. A 1 O is an oxygen alkyl group having 2 to 4 carbon atoms, and m is an integer of 0 to 15. n is an integer from 1 to 2. M 1 is a hydrogen atom, an alkali metal, an ammonium group or an organic amine group. Q 1 is M 1 or R 1 O(A 1 O) m . Y is 1 or 2.
作為R1的烴基,可以舉出:烷基、烯基等。R1的碳原子數較佳為8至24,更佳為12至24。R1的碳原子可以具有分布,R1可以為直鏈狀或具有支鏈者,亦可以是飽和或不飽和者。 Examples of the hydrocarbon group of R 1 include an alkyl group and an alkenyl group. The number of carbon atoms of R 1 is preferably from 8 to 24, more preferably from 12 to 24. The carbon atom of R 1 may have a distribution, and R 1 may be linear or branched, or may be saturated or unsaturated.
A1O為碳原子數2至4的氧伸烷基。氧伸烷基單元的重複數m為0至15的整數,較佳為0至10,更佳為0至 3,特佳係m為0即不含聚氧伸烷基的情況。(A1O)m較佳係具有作為氧伸烷基單元之氧伸乙基50莫耳%以上的聚氧伸烷基。 A 1 O is an oxygen-extended alkyl group having 2 to 4 carbon atoms. The repeating number m of the oxygen alkyl unit is an integer of from 0 to 15, preferably from 0 to 10, more preferably from 0 to 3, and particularly preferably m is 0, i.e., does not contain a polyoxyalkylene group. (A 1 O) m is preferably a polyoxyalkylene group having an oxygen extension ethyl group of 50 mol% or more as an oxygen alkyl unit.
n為1至2的整數。在n=2的情況下,構成由上述通式(2)表示的化合物的2個有機基「R1O(A1O)m]可為相同或相異。 n is an integer from 1 to 2. In the case of n=2, the two organic groups "R 1 O(A 1 O) m ] constituting the compound represented by the above formula (2) may be the same or different.
另外,在Q=R1O(A1O)m的情況下,構成由通式(3)表示的化合物的2個有機基「R1O(A1O)m」可為相同或相異。 Further, when Q = R 1 O(A 1 O) m , the two organic groups "R 1 O(A 1 O) m " constituting the compound represented by the general formula (3) may be the same or different .
M1為氫原子、鹼金屬、銨基或有機胺基。作為鹼金屬,例如可以列舉:鋰、鈉、鉀等。作為銨基及有機胺基,可以舉出:由NRaRbRcRd表示的基。由NRaRbRcRd表示的基與在有機磺酸化合物(B)處說明的M相同。 M 1 is a hydrogen atom, an alkali metal, an ammonium group or an organic amine group. Examples of the alkali metal include lithium, sodium, potassium, and the like. Examples of the ammonium group and the organic amine group include a group represented by NR a R b R c R d . The group represented by NR a R b R c R d is the same as M described at the organic sulfonic acid compound (B).
有機磷酸酯化合物(C)較佳係包含通式(2)中n=1時表示的有機磷酸酯化合物(C1)及通式(2)中n=2時表示的有機磷酸酯化合物(C2)而成的混合物、或者包含有機磷酸酯化合物(C1)、(C2)及通式(3)中Y=1、Q=R1O(A1O)m時表示的有機磷酸酯化合物(C3)而成的混合物。此等混合物中,亦可以含有通式(3)中Y=1、Q=氫原子時表示的有機磷酸酯化合物(C4)。 The organophosphate compound (C) preferably contains the organophosphate compound (C1) represented by n=1 in the formula (2) and the organophosphate compound (C2) represented by n=2 in the formula (2). The organic phosphate compound (C3) represented by the mixture or the organic phosphate compound (C1), (C2) and Y=1 in the general formula (3) and Q=R 1 O(A 1 O) m a mixture of. These mixtures may also contain an organic phosphate compound (C4) represented by Y = 1 in the general formula (3) and Q = a hydrogen atom.
有機磷酸酯化合物(C1)、(C2)、(C3)及(C4)以及無機磷酸的P核積分比例(%)能夠根據31P-NMR中來自各磷原子的譜峰的積分值進行計算。此外,P核積分比率(%)是指將有機磷酸酯化合物(C1)、(C2)、(C3)、(C4)及無機磷酸的積分值的合計以100%的形式算出的值。關於無機 磷酸係在後述。 The P-nucleus integral ratio (%) of the organophosphate compounds (C1), (C2), (C3), and (C4) and the inorganic phosphoric acid can be calculated from the integrated value of the peaks derived from the respective phosphorus atoms in the 31 P-NMR. In addition, the P core integral ratio (%) is a value calculated as a total of integrated values of the organic phosphate compounds (C1), (C2), (C3), (C4), and inorganic phosphoric acid in the form of 100%. The inorganic phosphate system will be described later.
有機磷酸酯化合物(C1)的P核積分比率(%)較佳為25至82%,更佳為35至80%,進一步更佳40至70%。有機磷酸酯化合物(C2)的P核積分比率(%)較佳為15至65%,更佳為20至60%,進一步更佳為25至55%。有機磷酸酯化合物(C3)的P核積分比率(%)較佳為0至50%,更佳為0至45%,進一步更佳為0至40%。有機磷酸酯化合物(C4)的P核積分比率(%)較佳為0至7%,更佳為0至6%,進一步更佳為0至5%。無機磷酸的P核積分比率(%)較佳為0至10%,更佳為0至9%,進一步更佳為0至8%。 The P core integral ratio (%) of the organophosphate compound (C1) is preferably from 25 to 82%, more preferably from 35 to 80%, still more preferably from 40 to 70%. The P core integral ratio (%) of the organophosphate compound (C2) is preferably from 15 to 65%, more preferably from 20 to 60%, still more preferably from 25 to 55%. The P core integral ratio (%) of the organophosphate compound (C3) is preferably from 0 to 50%, more preferably from 0 to 45%, still more preferably from 0 to 40%. The P core integral ratio (%) of the organophosphate compound (C4) is preferably from 0 to 7%, more preferably from 0 to 6%, still more preferably from 0 to 5%. The P core integral ratio (%) of the inorganic phosphoric acid is preferably from 0 to 10%, more preferably from 0 to 9%, still more preferably from 0 to 8%.
作為有機磷酸酯化合物(C)的製造方法,沒有特別限定,可以採用公知的方法。例如,有機磷酸酯化合物(C)的製造方法包括使由R1O(A1O)mH表示的有機羥基化合物與磷酸酐P2O5反應而得到反應物的步驟(I)。此外,在步驟(I)中,亦可以加入無機磷酸、水來進行反應。有機磷酸酯化合物(C)的製造方法亦可以包含在步驟(I)之後將水添加至前述反應物中而進行水解的步驟(II)。藉由包括步驟(II),從而能夠調整有機磷酸酯化合物(C)中所含有的有機磷酸酯化合物(C3)、(C4)的比率。相對於上述有機磷酸酯化合物(C),添加至上述反應物中的水的量較佳為0.01至5重量%,更佳為0.05至4重量%,進一步更佳為0.1至3重量%。如果水的添加量小於0.01重量%或超過5重量%,則存在有難以調節有機磷酸酯化合物(C3)、(C4)的量的情況。作為有機磷酸酯化合物(C)的製造方法,亦可以在步驟 (I)或步驟(II)之後包括用具有M1的鹼性化合物進行中和的步驟(III)。 The method for producing the organophosphate compound (C) is not particularly limited, and a known method can be employed. For example, the method for producing the organophosphate compound (C) includes the step (I) of reacting an organic hydroxy compound represented by R 1 O(A 1 O) m H with phosphoric anhydride P 2 O 5 to obtain a reactant. Further, in the step (I), inorganic phosphoric acid or water may be added to carry out the reaction. The method for producing the organophosphate compound (C) may further comprise the step (II) of adding water to the above reactant after the step (I) to carry out hydrolysis. By including the step (II), the ratio of the organic phosphate compounds (C3) and (C4) contained in the organophosphate compound (C) can be adjusted. The amount of water added to the above reactant is preferably from 0.01 to 5% by weight, more preferably from 0.05 to 4% by weight, still more preferably from 0.1 to 3% by weight, based on the above organophosphate compound (C). If the amount of water added is less than 0.01% by weight or more than 5% by weight, there is a case where it is difficult to adjust the amounts of the organic phosphate compounds (C3) and (C4). As a method for producing the organophosphate compound (C), the step (III) of neutralizing with a basic compound having M 1 may be included after the step (I) or the step (II).
有機磷酸酯化合物(C)中包含作為磷酸酐或無機磷中的雜質來源的砷等的重金屬化合物。本發明的處理劑亦可以含有砷等的重金屬化合物。從對人體的影響或對環境的安全性的觀點考慮,重金屬化合物在處理劑的不揮發成分中所佔的重量比率較佳為0.01重量%以下,更佳為0.005重量%以下,進一步更佳為0.001重量%以下。 The organophosphate compound (C) contains a heavy metal compound such as arsenic or the like which is a source of impurities in phosphoric anhydride or inorganic phosphorus. The treatment agent of the present invention may also contain a heavy metal compound such as arsenic. The weight ratio of the heavy metal compound to the nonvolatile matter of the treating agent is preferably 0.01% by weight or less, more preferably 0.005% by weight or less, further preferably more preferably, from the viewpoint of the influence on the human body or the safety of the environment. 0.001% by weight or less.
在製造有機磷酸酯化合物(C)時,會產生無機磷酸及/或其鹽。因此,包含有機磷酸酯化合物(C)的原料(以下,稱為原料Z)中含有無機磷酸及/或其鹽。無機磷酸及/或其鹽的比率能夠藉由有機羥基化合物與磷酸酐P2O5的比例、反應條件等進行調整。 In the production of the organic phosphate compound (C), inorganic phosphoric acid and/or a salt thereof is produced. Therefore, the raw material containing the organophosphate compound (C) (hereinafter referred to as the raw material Z) contains inorganic phosphoric acid and/or a salt thereof. The ratio of the inorganic phosphoric acid and/or its salt can be adjusted by the ratio of the organic hydroxy compound to the phosphoric anhydride P 2 O 5 , the reaction conditions, and the like.
本發明的處理劑,從賦予原絲油膜强度、集束性並提高制紗性的觀點考慮,除了上述平滑成分(A)、有機磺酸化合物(B)之外,較佳係更含有非離子界面活性劑(D)。此外,非離子界面活性劑(D)是指除了上述平滑成分(A)以外者。非離子界面活性劑(D)可以使用1種或2種以上。 The treatment agent of the present invention preferably contains a nonionic interface in addition to the smooth component (A) and the organic sulfonic acid compound (B) from the viewpoint of imparting strength and bundling properties of the strand oil film and improving yarn-making property. Active agent (D). Further, the nonionic surfactant (D) means aside from the above smoothing component (A). The nonionic surfactant (D) may be used alone or in combination of two or more.
作為非離子界面活性劑(D),可以舉出:含有聚氧伸烷基的羥基脂肪酸多元醇酯(以下,有時稱為聚羥基酯)、將聚羥基酯中的至少一個羥基用脂肪酸封端而成的酯、聚環氧烷(polyoxyalkylene)多元醇醚、聚環氧烷多元醇 脂肪酸酯、聚環氧烷脂肪族醇醚、聚烷二醇的脂肪酸酯、多元醇脂肪酸酯等。 Examples of the nonionic surfactant (D) include a polyhydroxyalkylene group-containing hydroxy fatty acid polyol ester (hereinafter sometimes referred to as a polyhydroxy ester), and at least one hydroxyl group in the polyhydroxy ester is sealed with a fatty acid. End-ester ester, polyoxyalkylene polyol ether, polyalkylene oxide polyol A fatty acid ester, a polyalkylene oxide aliphatic alcohol ether, a fatty acid ester of a polyalkylene glycol, a polyhydric alcohol fatty acid ester, or the like.
聚羥基酯較佳在結構上是含有聚氧伸烷基的羥基脂肪酸與多元醇的酯,較佳係多元醇的羥基中的2個以上的羥基被酯化。因此,含有聚氧伸烷基的羥基脂肪酸多元醇酯係具有複數個羥基的酯。 The polyhydroxy ester is preferably an ester of a polyhydroxyalkylene group-containing hydroxy fatty acid and a polyhydric alcohol. Preferably, two or more hydroxyl groups in the hydroxyl group of the polyhydric alcohol are esterified. Therefore, the hydroxy fatty acid polyol ester containing a polyoxyalkylene group has an ester having a plurality of hydroxyl groups.
含有聚氧伸烷基的羥基脂肪酸係於脂肪酸的烴基上具有透過氧原子而鍵結有聚氧伸烷基的結構,並且聚氧伸烷基的不與脂肪酸的烴基鍵結的一個末端成為羥基。 The hydroxy fatty acid having a polyoxyalkylene group has a structure in which a polyoxyalkylene group is bonded to an oxygen atom on a hydrocarbon group of a fatty acid, and a terminal end of the polyoxyalkylene group which is not bonded to a hydrocarbon group of the fatty acid is a hydroxyl group. .
作為聚羥基酯,例如可以列舉:碳原子數6至22(較佳為16至20)的羥基脂肪酸與多元醇的酯化物的環氧烷(alkylene oxide)加成物。 The polyhydroxy ester may, for example, be an alkylene oxide adduct of an esterified product of a hydroxy fatty acid having 6 to 22 (preferably 16 to 20) carbon atoms and a polyhydric alcohol.
作為碳原子數6至22的羥基脂肪酸,例如可以舉出:羥基辛酸、羥基癸酸、羥基月桂酸、羥基硬脂酸、蓖麻醇酸,較佳為羥基十八烷酸、蓖麻醇酸。作為多元醇,例如可以舉出:乙二醇、甘油、山梨糖醇、脫水山梨糖醇、三羥甲基丙烷、新戊四醇等,較佳為甘油。作為環氧烷,可以舉出:環氧乙烷、環氧丙烷、環氧丁烷等碳原子數為2至4的環氧烷。 Examples of the hydroxy fatty acid having 6 to 22 carbon atoms include hydroxyoctanoic acid, hydroxydecanoic acid, hydroxylauric acid, hydroxystearic acid, and ricinoleic acid, preferably hydroxyoctadecanoic acid and ricinoleic acid. . Examples of the polyhydric alcohol include ethylene glycol, glycerin, sorbitol, sorbitan, trimethylolpropane, and pentaerythritol, and glycerin is preferred. The alkylene oxide may, for example, be an alkylene oxide having 2 to 4 carbon atoms such as ethylene oxide, propylene oxide or butylene oxide.
環氧烷的加成莫耳數較佳為3至60,更佳 為8至50。環氧乙烷在環氧烷中所佔的比率較佳為50莫耳%,更佳為80莫耳%。 The addition mole number of the alkylene oxide is preferably from 3 to 60, more preferably It is 8 to 50. The ratio of ethylene oxide in the alkylene oxide is preferably 50 mol%, more preferably 80 mol%.
在加成2種以上環氧烷的情況下,此等的加成順序沒有特別限定,加成形態可以是嵌段狀、隨機狀中的任一者。環氧烷的加成可以藉由公知的方法進行,但通常是在鹼性催化劑的存在下進行。 In the case of adding two or more kinds of alkylene oxides, the order of addition is not particularly limited, and the addition form may be either a block form or a random form. The addition of the alkylene oxide can be carried out by a known method, but it is usually carried out in the presence of a basic catalyst.
聚羥基酯係可以如下方式製造,例如:在通常條件下,將多元醇與羥基脂肪酸(羥基單羧酸)酯化而得到酯化物,接著使環氧烷與該酯化物進行加成反應而製造。聚羥基酯也可以藉由如下方式來適當地製造,如:使用蓖麻油等天然得到的油脂或在其中添加氫而成的氫化蓖麻油,然後與環氧烷進行加成反應而得到。 The polyhydroxy ester system can be produced, for example, by esterifying a polyhydric alcohol with a hydroxy fatty acid (hydroxy monocarboxylic acid) under ordinary conditions to obtain an esterified product, followed by addition reaction of an alkylene oxide and the esterified product. . The polyhydroxy ester can also be suitably produced, for example, by using a naturally occurring fat or oil such as castor oil or hydrogenated castor oil obtained by adding hydrogen thereto, followed by addition reaction with alkylene oxide.
非離子界面活性劑(D)中亦含有上述的將聚羥基酯中的至少一個羥基用脂肪酸封端而成的酯。封端的脂肪酸的碳原子數較佳為6至24,更佳為12至18。脂肪酸中的烴基的碳原子數可以具有分布,烴基可為直鏈狀或具有支鏈者,亦可為飽和或不飽和者,也可以具有多環的結構。作為如此的脂肪酸,例如可以舉出:月桂酸、肉豆蔻酸、棕櫚酸、棕櫚油酸、硬脂酸、油酸、二十烷酸、二十二烷酸、二十四烷酸等。對於酯化的方法、反應條件等沒有特別限定,能夠使用公知的方法、通常的條件。 The nonionic surfactant (D) also contains the above-mentioned ester in which at least one of the polyhydroxy esters is blocked with a fatty acid. The blocked fatty acid preferably has 6 to 24 carbon atoms, more preferably 12 to 18 carbon atoms. The hydrocarbon group in the fatty acid may have a distribution of carbon atoms, and the hydrocarbon group may be linear or branched, or may be saturated or unsaturated, or may have a polycyclic structure. Examples of such a fatty acid include lauric acid, myristic acid, palmitic acid, palmitoleic acid, stearic acid, oleic acid, eicosanoic acid, behenic acid, and tetracosanoic acid. The method of esterification, the reaction conditions, and the like are not particularly limited, and a known method and usual conditions can be used.
作為聚羥基酯以及將聚羥基酯中的至少一個羥基用脂肪酸封端而成的酯,例如是氫化蓖麻油環氧乙烷加成物、蓖麻油環氧乙烷加成物、氫化蓖麻油環氧乙烷 加成物單油酸酯、氫化蓖麻油環氧乙烷加成物二油酸酯、氫化蓖麻油環氧乙烷加成物三油酸酯、蓖麻油環氧乙烷加成物三油酸酯、氫化蓖麻油環氧乙烷加成物三硬脂酸酯、蓖麻油環氧乙烷加成物三硬脂酸酯,其中,從處理劑的相溶性、油膜强度、絨毛減少的觀點考慮,較佳為氫化蓖麻油環氧乙烷加成物、氫化蓖麻油環氧乙烷加成物三油酸酯、氫化蓖麻油環氧乙烷加成物三硬脂酸酯。 As the polyhydroxy ester and an ester obtained by blocking at least one hydroxyl group in the polyhydroxy ester with a fatty acid, for example, hydrogenated castor oil ethylene oxide adduct, castor oil ethylene oxide adduct, hydrogenated castor oil ring Oxyethane Addition monooleate, hydrogenated castor oil ethylene oxide adduct dioleate, hydrogenated castor oil ethylene oxide adduct trioleate, castor oil ethylene oxide adduct trioleate Ester, hydrogenated castor oil ethylene oxide adduct tristearate, castor oil ethylene oxide adduct tristearate, from the viewpoint of compatibility of the treating agent, oil film strength, and fluff reduction Preferred are hydrogenated castor oil ethylene oxide adduct, hydrogenated castor oil ethylene oxide adduct trioleate, hydrogenated castor oil ethylene oxide adduct tristearate.
聚環氧烷多元醇醚是指於多元醇上具有加成有環氧乙烷、環氧丙烷、環氧丁烷等環氧烷而成的結構的化合物。 The polyalkylene oxide polyol ether is a compound having a structure in which an alkylene oxide such as ethylene oxide, propylene oxide or butylene oxide is added to the polyol.
作為多元醇,可以舉出:乙二醇、甘油、三羥甲基丙烷、新戊四醇、二甘油、脫水山梨糖醇、山梨糖醇、二三羥甲基丙烷、二新戊四醇、蔗糖等。其中,較佳為甘油、三羥甲基丙烷、蔗糖。 Examples of the polyhydric alcohol include ethylene glycol, glycerin, trimethylolpropane, pentaerythritol, diglycerin, sorbitan, sorbitol, ditrimethylolpropane, and dipentaerythritol. Sucrose and the like. Among them, glycerin, trimethylolpropane, and sucrose are preferred.
作為環氧烷的加成莫耳數,較佳為3至100,更佳為4至70,進一步更佳為5至50。此外,環氧乙烷在環氧烷中所佔的比率較佳為50莫耳%以上,更佳為80莫耳%以上。 The addition mole number of the alkylene oxide is preferably from 3 to 100, more preferably from 4 to 70, still more preferably from 5 to 50. Further, the ratio of ethylene oxide to alkylene oxide is preferably 50 mol% or more, more preferably 80 mol% or more.
聚環氧烷多元醇醚的重量平均分子量較佳為300至10000,更佳為400至8000,進一步更佳為500至5000。在該分子量小於300時,無法減少絨毛、斷紗的產生。另一方面,該分子量超過10000時,則處理劑的摩擦變高,不僅無法減少絨毛、斷紗的發生,而且還會使其惡化。 The polyalkylene oxide polyol ether preferably has a weight average molecular weight of from 300 to 10,000, more preferably from 400 to 8,000, still more preferably from 500 to 5,000. When the molecular weight is less than 300, the generation of fluff and yarn breakage cannot be reduced. On the other hand, when the molecular weight exceeds 10,000, the friction of the treatment agent becomes high, and it is not only impossible to reduce the occurrence of fluff and yarn breakage, but also to deteriorate it.
作為聚環氧烷多元醇醚,可以舉出:聚乙二醇、甘油環氧乙烷加成物、三羥甲基丙烷環氧乙烷加成物、新戊四醇環氧乙烷加成物、二甘油環氧乙烷加成物、山梨糖醇酐環氧乙烷加成物、山梨糖醇酐環氧乙烷環氧丙烷加成物、山梨糖醇環氧乙烷加成物、山梨糖醇環氧乙烷環氧丙烷加成物、二三羥甲基丙烷環氧乙烷加成物、二新戊四醇環氧乙烷加成物、蔗糖環氧乙烷加成物等,但不限於此。 Examples of the polyalkylene oxide polyol ether include polyethylene glycol, glycerin ethylene oxide adduct, trimethylolpropane ethylene oxide adduct, and neopentyl alcohol ethylene oxide addition. , diglycerin ethylene oxide adduct, sorbitan ethylene oxide adduct, sorbitan oxide ethylene oxide propylene oxide adduct, sorbitol ethylene oxide adduct, Sorbitol ethylene oxide propylene oxide adduct, ditrimethylolpropane ethylene oxide adduct, dipentaerythritol ethylene oxide adduct, sucrose ethylene oxide adduct, etc. , but not limited to this.
聚環氧烷多元醇脂肪酸酯係於多元醇上具有加成有環氧乙烷、環氧丙烷、環氧丁烷等環氧烷而成的化合物與脂肪酸所形成的酯鍵結構的化合物。 The polyalkylene oxide polyol fatty acid ester is a compound having an ester bond structure formed by a compound obtained by adding an alkylene oxide such as ethylene oxide, propylene oxide or butylene oxide to a polyhydric alcohol.
作為多元醇,可以舉出:甘油、三羥甲基丙烷、新戊四醇、赤蘚醇、二甘油、脫水山梨糖醇、山梨糖醇、二三羥甲基丙烷、二新戊四醇、蔗糖等。其中,較佳為甘油、二甘油、脫水山梨糖醇、山梨糖醇。 Examples of the polyhydric alcohol include glycerin, trimethylolpropane, neopentyl alcohol, erythritol, diglycerin, sorbitan, sorbitol, ditrimethylolpropane, and dipentaerythritol. Sucrose and the like. Among them, glycerin, diglycerin, sorbitan, and sorbitol are preferred.
作為脂肪酸,可以舉出:月桂酸、肉豆蔻酸、肉豆蔻油酸、棕櫚酸、棕櫚油酸、異鯨蠟酸、硬脂酸、異硬脂酸、油酸、反式油酸、亞油酸、亞麻酸、花生酸、二十烯酸、二十二烷酸、異二十二碳酸、順芥子酸、二十四烷酸、異二十四烷酸等。 Examples of the fatty acid include lauric acid, myristic acid, myristic acid, palmitic acid, palmitoleic acid, isoctanic acid, stearic acid, isostearic acid, oleic acid, trans-oleic acid, and linoleic acid. Acid, linolenic acid, arachidic acid, eicosenoic acid, behenic acid, iso-docosaic acid, erucic acid, tetracosanoic acid, isotetradecanoic acid and the like.
作為環氧烷的加成莫耳數,較佳為3至100,更佳為5至70,進一步更佳為10至50。此外,環氧 乙烷在環氧烷中所佔的比率較佳為50莫耳%以上,更佳為80莫耳%以上。 The addition mole number of the alkylene oxide is preferably from 3 to 100, more preferably from 5 to 70, still more preferably from 10 to 50. In addition, epoxy The ratio of ethane in the alkylene oxide is preferably 50 mol% or more, more preferably 80 mol% or more.
聚環氧烷多元醇脂肪酸酯的重量平均分子量較佳為300至7000,更佳為500至5000,進一步更佳為700至3000。在該分子量小於300時,會有在熱處理步驟中發生冒煙,而使環境惡化的情況。此外,無法降低斷紗的發生。另一方面,該分子量超過7000時,則處理劑的摩擦增大,不但無法夠降低絨毛、斷紗的產生,反而會使其惡化。 The polyalkylene oxide polyol fatty acid ester preferably has a weight average molecular weight of from 300 to 7,000, more preferably from 500 to 5,000, still more preferably from 700 to 3,000. When the molecular weight is less than 300, there is a case where smoke is generated in the heat treatment step and the environment is deteriorated. In addition, the occurrence of yarn breakage cannot be reduced. On the other hand, when the molecular weight exceeds 7,000, the friction of the treatment agent increases, and the occurrence of fluff and yarn breakage cannot be reduced, and the deterioration is caused.
作為聚環氧烷多元醇脂肪酸酯,可以舉出:甘油環氧乙烷加成物單月桂酸酯、甘油環氧乙烷加成物二月桂酸酯、甘油環氧乙烷加成物三月桂酸酯、三羥甲基丙烷環氧乙烷加成物三月桂酸酯、脫水山梨糖醇環氧乙烷加成物單油酸酯、脫水山梨糖醇環氧乙烷加成物二油酸酯、脫水山梨糖醇環氧乙烷加成物三油酸酯、脫水山梨糖醇環氧乙烷環氧丙烷加成物單油酸酯、脫水山梨糖醇環氧乙烷環氧丙烷加成物二油酸酯、脫水山梨糖醇環氧乙烷環氧丙烷加成物三油酸酯、脫水山梨糖醇環氧乙烷環氧丙烷加成物三月桂酸酯、蔗糖環氧乙烷加成物三月桂酸酯等,但不限於此。 Examples of the polyalkylene oxide polyol fatty acid ester include glycerin ethylene oxide adduct monolaurate, glycerin ethylene oxide adduct dilaurate, and glycerin ethylene oxide adduct. Lauric acid ester, trimethylolpropane ethylene oxide adduct trilaurate, sorbitan ethylene oxide adduct monooleate, sorbitan ethylene oxide adduct Acid ester, sorbitan ethylene oxide adduct trioleate, sorbitan ethylene oxide propylene oxide adduct monooleate, sorbitan ethylene oxide propylene oxide Compound dioleate, sorbitan oxide ethylene oxide propylene oxide adduct trioleate, sorbitan ethylene oxide propylene oxide adduct trilaurate, sucrose ethylene oxide The adduct trilaurate or the like is not limited thereto.
聚環氧烷脂肪族醇醚係於脂肪族一元醇上具有加成有環氧乙烷、環氧丙烷、環氧丁烷等環氧烷而成的結構的化合物。 The polyalkylene oxide aliphatic alcohol ether is a compound having a structure in which an alkylene oxide such as ethylene oxide, propylene oxide or butylene oxide is added to an aliphatic monohydric alcohol.
作為聚環氧烷脂肪族醇醚,例如可以舉出:辛醇、2-乙基己醇、癸醇、月桂醇、十三烷基醇、肉豆蔻醇、硬脂醇、異硬脂醇、油醇等脂肪族醇的環氧烷加成物。 Examples of the polyalkylene oxide aliphatic alcohol ether include octanol, 2-ethylhexanol, decyl alcohol, lauryl alcohol, tridecyl alcohol, myristyl alcohol, stearyl alcohol, and isostearyl alcohol. An alkylene oxide adduct of an aliphatic alcohol such as oleyl alcohol.
作為環氧烷的加成莫耳數,較佳為1至100莫耳,更佳為2至70莫耳,進一步更佳為3至50莫耳。此外,環氧乙烷相對於環氧烷整體的比例較佳為20莫耳%以上,更佳為30莫耳%以上,進一步更佳為40莫耳%以上。 The addition mole number of the alkylene oxide is preferably from 1 to 100 moles, more preferably from 2 to 70 moles, still more preferably from 3 to 50 moles. Further, the ratio of ethylene oxide to the entire alkylene oxide is preferably 20 mol% or more, more preferably 30 mol% or more, still more preferably 40 mol% or more.
聚烷二醇的脂肪酸酯是指具有聚氧乙二醇(polyoxyethylene glycol)、聚氧乙烯聚氧丙烯二醇(polyoxyethylene polyoxypropylene glycol)與脂肪酸所形成的酯鍵結構的化合物。聚烷二醇的重量平均分子量較佳為100至1000,更佳為150至800,進一步更佳為200至700。 The fatty acid ester of a polyalkylene glycol is a compound having an ester bond structure formed of polyoxyethylene glycol, polyoxyethylene polyoxypropylene glycol, and a fatty acid. The weight average molecular weight of the polyalkylene glycol is preferably from 100 to 1,000, more preferably from 150 to 800, still more preferably from 200 to 700.
作為聚烷二醇脂肪酸酯,可以舉出:聚乙二醇單月桂酸酯、聚乙二醇二月桂酸酯、聚乙二醇單油酸酯、聚乙二醇二油酸酯、聚乙二醇單硬脂酸酯、聚乙二醇二硬脂酸酯、聚乙烯聚丙二醇單月桂酸酯、聚乙烯聚丙烯二醇二月桂酸酯、聚乙烯聚丙烯二醇單油酸酯、聚乙烯聚丙烯二醇二油酸酯等,但不限於此。 Examples of the polyalkylene glycol fatty acid ester include polyethylene glycol monolaurate, polyethylene glycol dilaurate, polyethylene glycol monooleate, polyethylene glycol dioleate, and poly Ethylene glycol monostearate, polyethylene glycol distearate, polyethylene polypropylene glycol monolaurate, polyethylene polypropylene glycol dilaurate, polyethylene polypropylene glycol monooleate, Polyethylene polypropylene glycol dioleate, etc., but is not limited thereto.
多元醇脂肪酸酯是具有多元醇與脂肪酸所形成的酯 鍵結構的化合物,是除了上述平滑成分(A)之外的化合物。 Polyol fatty acid esters are esters formed from polyols and fatty acids The compound having a bond structure is a compound other than the above smoothing component (A).
作為多元醇,可以舉出:乙二醇、三羥甲基丙烷、新戊四醇、赤蘚醇、二乙二醇、二甘油、脫水山梨糖醇、山梨糖醇、二三羥甲基丙烷、蔗糖等。其中,較佳為乙二醇、甘油、二甘油、脫水山梨糖醇、山梨糖醇。 Examples of the polyhydric alcohol include ethylene glycol, trimethylolpropane, neopentyl alcohol, erythritol, diethylene glycol, diglycerin, sorbitan, sorbitol, and ditrimethylolpropane. , sucrose, etc. Among them, preferred are ethylene glycol, glycerin, diglycerin, sorbitan, and sorbitol.
作為脂肪酸,可以舉出:月桂酸、肉豆蔻酸、肉豆蔻油酸、棕櫚酸、棕櫚油酸、異鯨蠟酸、硬脂酸、異硬脂酸、油酸、反式油酸、亞油酸、亞麻酸、結核硬脂酸、異二十碳酸、鱈油酸、二十烯酸、二十二烷酸、異二十二烷酸、順芥子酸、二十四烷酸等。 Examples of the fatty acid include lauric acid, myristic acid, myristic acid, palmitic acid, palmitoleic acid, isoctanic acid, stearic acid, isostearic acid, oleic acid, trans-oleic acid, and linoleic acid. Acid, linolenic acid, tuberculous stearic acid, isodecanoic acid, oleic acid, eicosenoic acid, behenic acid, isodocosalic acid, erucic acid, tetracosanoic acid and the like.
而且,該多元醇脂肪酸酯係至少具有1個或2個以上的羥基。 Further, the polyol fatty acid ester has at least one or two or more hydroxyl groups.
多元醇脂肪酸酯的重量平均分子量較佳為100至1000,更佳為200至800,進一步更佳為300至600。 The weight average molecular weight of the polyol fatty acid ester is preferably from 100 to 1,000, more preferably from 200 to 800, still more preferably from 300 to 600.
作為脂肪酸酯,可以舉出:甘油單月桂酸酯、甘油二月桂酸酯、甘油單油酸酯、甘油二油酸酯、山梨糖醇酐單油酸酯、脫水山梨糖醇二油酸酯、蔗糖單月桂酸酯、蔗糖二月桂酸酯等,但不限於此。 Examples of the fatty acid esters include glycerin monolaurate, glycerin dilaurate, glycerin monooleate, glyceryl dioleate, sorbitan monooleate, and sorbitan dioleate. , sucrose monolaurate, sucrose dilaurate, etc., but are not limited thereto.
作為非離子界面活性劑(D),從提高耐熱性的觀點考慮,較佳係使用除去催化劑等並精製過者。 The nonionic surfactant (D) is preferably purified by removing a catalyst or the like from the viewpoint of improving heat resistance.
本發明的處理劑是含有平滑成分(A)與由上述通式(1)表示的有機磺酸化合物(B)者。並且,藉由離子色譜法從處 理劑的不揮發成分中檢測出的硫酸根離子(SO4 2-)的重量比率為200ppm以下,並且氯離子(Cl-)的重量比率為200ppm以下。如此,藉由將從處理劑的不揮發成分中檢測出的硫酸根離子與氯離子設定為規定的重量比率以下,從而能夠急劇降低絨毛、斷紗、輥污染。 The treatment agent of the present invention is a compound containing the smoothing component (A) and the organic sulfonic acid compound (B) represented by the above formula (1). Further, the weight ratio of sulfate ion (SO 4 2- ) detected from the nonvolatile matter of the treatment agent by ion chromatography is 200 ppm or less, and the weight ratio of chloride ion (Cl - ) is 200 ppm or less. By setting the sulfate ion and the chloride ion detected from the non-volatile component of the treatment agent to a predetermined weight ratio or less, it is possible to drastically reduce fluff, yarn breakage, and roll contamination.
在該硫酸根離子的重量比率超過200ppm時或該氯離子的重量比率超過200ppm時,硫酸鈉、氯化鈉在紡紗時會脫落並累積在拉伸輥上,引起斷線斷紗的增加,對於進行熱拉伸的輥,加快焦油的累積,引起輥污染。 When the weight ratio of the sulfate ion exceeds 200 ppm or the weight ratio of the chloride ion exceeds 200 ppm, sodium sulfate and sodium chloride may fall off during the spinning and accumulate on the stretching roll, causing an increase in broken yarn breakage. For rolls that are hot drawn, the accumulation of tar is accelerated, causing roll contamination.
此外,本發明中的藉由離子色譜法所進行的硫酸根離子、氯離子的分析方法,係按照實施例中記載的內容。此外,本發明中的不揮發成分是指以105℃將處理劑進行熱處理而除去溶劑等後,達到恆重時的絕對乾燥成分。 Further, the method for analyzing sulfate ions and chloride ions by ion chromatography in the present invention is as described in the examples. In addition, the non-volatile component in the present invention refers to an absolute dry component when the treatment agent is heat-treated at 105 ° C to remove a solvent or the like and reaches a constant weight.
從更發揮本發明的效果的觀點考慮,該硫酸根離子的重量比率較佳為200ppm以下,更佳為150ppm以下,進一步更佳為100ppm以下。同樣,該氯離子的重量比率較佳為200ppm以下,更佳為150ppm以下,進一步更佳為100ppm以下。 The weight ratio of the sulfate ion is preferably 200 ppm or less, more preferably 150 ppm or less, still more preferably 100 ppm or less from the viewpoint of further exerting the effects of the present invention. Similarly, the weight ratio of the chloride ion is preferably 200 ppm or less, more preferably 150 ppm or less, still more preferably 100 ppm or less.
作為硫酸根離子及氯離子的重量比率的調整方法,如前所述,可藉由降低在包含有機磺酸化合物(B)的原料X中所含有的硫酸鈉、氯化鈉來實現。 The method of adjusting the weight ratio of the sulfate ion and the chloride ion can be achieved by reducing sodium sulfate or sodium chloride contained in the raw material X containing the organic sulfonic acid compound (B) as described above.
平滑成分(A)在處理劑的不揮發成分中所佔的重量比率較佳為20至70重量%,更佳為30至65重量%,進一步更佳為40至65重量%,特佳為40至60重量%。在 該重量比率小於20重量%時,有時會因平滑性不足而造成絨毛增加。另一方面,在該重量比率超過70重量%時,會有集束性不足,或在乳化使用的情況下,有可能乳化穩定性變差而無法使用。 The weight ratio of the smoothing component (A) to the nonvolatile content of the treating agent is preferably from 20 to 70% by weight, more preferably from 30 to 65% by weight, still more preferably from 40 to 65% by weight, particularly preferably 40. Up to 60% by weight. in When the weight ratio is less than 20% by weight, the pile may be increased due to insufficient smoothness. On the other hand, when the weight ratio exceeds 70% by weight, the bundleability may be insufficient, or in the case of emulsification, the emulsion stability may be deteriorated and it may be unusable.
有機磺酸化合物(B)在處理劑的不揮發成分中所佔的重量比率為1.25至12重量%,較佳為1.25至10重量%,更佳為1.25至8重量%,進一步更佳為1.25至7重量%,特佳為1.5至6重量%。在該重量比率小於1.25重量%時,有時無法降低輥污染。另一方面,在該重量比率超過12重量%時,會摩擦增加而使絨毛增加。 The organic sulfonic acid compound (B) accounts for 1.25 to 12% by weight, preferably 1.25 to 10% by weight, more preferably 1.25 to 8% by weight, still more preferably 1.25, based on the nonvolatile content of the treating agent. Up to 7% by weight, particularly preferably from 1.5 to 6% by weight. When the weight ratio is less than 1.25 wt%, roll contamination may not be reduced. On the other hand, when the weight ratio exceeds 12% by weight, the friction increases and the pile increases.
在本發明的處理劑含有有機磷酸酯化合物(C)的情況下,藉由離子色譜法從處理劑的不揮發成分中檢測出的磷酸根離子(PO4 3-)的重量比率較佳為500ppm以下。在該磷酸根離子的重量比率超過500ppm時,有可能脫落在拉伸輥上而引起斷線斷紗的增加之虞。該磷酸根離子的重量比率更佳為400ppm以下,進一步更佳為300ppm以下,特別較佳為200ppm以下。此外,有時將磷酸根離子(PO4 3-)簡稱為磷酸根離子。 In the case where the treating agent of the present invention contains the organic phosphate compound (C), the weight ratio of the phosphate ion (PO 4 3- ) detected from the nonvolatile matter of the treating agent by ion chromatography is preferably 500 ppm. the following. When the weight ratio of the phosphate ion exceeds 500 ppm, there is a possibility that it falls off on the stretching roll to cause an increase in the yarn breakage. The weight ratio of the phosphate ion is more preferably 400 ppm or less, still more preferably 300 ppm or less, and particularly preferably 200 ppm or less. Further, a phosphate ion (PO 4 3- ) is sometimes simply referred to as a phosphate ion.
作為磷酸根離子的重量比率的調整方法,如前所述,可以藉由降低在包含有機磷酸酯化合物(C)的原料Z中所含有的無機磷酸及/或其鹽、或調整原料Z的配合量,使用矽藻土等過濾助劑過濾處理劑來實現。 As a method of adjusting the weight ratio of the phosphate ions, as described above, the inorganic phosphate and/or its salt contained in the raw material Z containing the organic phosphate compound (C) can be reduced, or the blending of the raw material Z can be adjusted. The amount is achieved by using a filter aid such as a filter aid such as diatomaceous earth.
在本發明的處理劑含有有機磷酸酯化合物(C)的情況下,有機磷酸酯化合物(C)在處理劑的不揮發成 分中所佔的重量比率較佳為0.05至10重量%,更佳為0.08至8重量%,進一步更佳為0.1至7重量%。 In the case where the treating agent of the present invention contains the organic phosphate compound (C), the organic phosphate compound (C) is not volatilized in the treating agent. The weight ratio in the portion is preferably from 0.05 to 10% by weight, more preferably from 0.08 to 8% by weight, still more preferably from 0.1 to 7% by weight.
在本發明的處理劑含有非離子界面活性劑(D)的情況下,非離子界面活性劑(D)在處理劑的不揮發成分中所佔的重量比率較佳為20至70重量%,更佳為25至65重量%,進一步更佳為30至65重量%,特佳為30至60重量%。 In the case where the treating agent of the present invention contains the nonionic surfactant (D), the weight ratio of the nonionic surfactant (D) to the nonvolatile component of the treating agent is preferably from 20 to 70% by weight, more It is preferably from 25 to 65% by weight, still more preferably from 30 to 65% by weight, particularly preferably from 30 to 60% by weight.
為了實現處理劑的乳化、對纖維的附著性輔助、來自纖維的處理劑的水洗、對纖維賦予制電性、潤滑性、集束性等,本發明的合成纖維用處理劑亦可以含有上述有機磺酸化合物(B)、有機磷酸酯化合物(C)及除了非離子界面活性劑(D)以外的界面活性劑。作為如此的界面活性劑,可以舉出脂肪酸肥皂等陰離子界面活性劑;烷基胺鹽、烷基咪唑鎓鹽、四級銨鹽等陽離子界面活性劑;月桂基二甲基甜菜鹼、硬脂基二甲基甜菜鹼等兩性界面活性劑;二甲基月桂基胺氧化物等。此等界面活性劑可以使用1種或2種以上。含有此等界面活性劑的情況下該界面活性劑在處理劑的不揮發成分中所佔的重量比率沒有特別限定,較佳為0.01至15重量%,更佳為0.1至10重量%。在此所指的界面活性劑是指重量平均分子量小於1000者。 The treatment agent for synthetic fibers of the present invention may contain the above organic sulfonate in order to achieve emulsification of the treatment agent, adhesion to the fibers, water washing of the treatment agent from the fibers, imparting electrical properties to the fibers, lubricity, and bundling properties. The acid compound (B), the organic phosphate compound (C), and a surfactant other than the nonionic surfactant (D). Examples of such a surfactant include an anionic surfactant such as a fatty acid soap; a cationic surfactant such as an alkylamine salt, an alkylimidazolium salt or a quaternary ammonium salt; lauryl dimethyl betaine and stearyl group; An amphoteric surfactant such as dimethyl betaine; dimethyl laurylamine oxide or the like. These surfactants may be used alone or in combination of two or more. In the case where such a surfactant is contained, the weight ratio of the surfactant to the nonvolatile component of the treating agent is not particularly limited, and is preferably from 0.01 to 15% by weight, more preferably from 0.1 to 10% by weight. By surfactant herein is meant a weight average molecular weight of less than 1000.
另外,為了賦予耐熱性,本發明的合成纖維用處理劑亦可以含有抗氧化劑。作為抗氧化劑,可以舉 出:苯酚系、硫系、亞磷酸酯系等公知的抗氧化劑。抗氧化劑可以使用1種或2種以上。在含有抗氧化劑的情況下,抗氧化劑在處理劑的不揮發成分中所佔的重量比率沒有特別限定,較佳為0.1至5重量%,宜為0.1至3重量%。 Further, in order to impart heat resistance, the treating agent for synthetic fibers of the present invention may contain an antioxidant. As an antioxidant, it can be A well-known antioxidant such as a phenol type, a sulfur type, or a phosphite type is mentioned. One type or two or more types of antioxidants can be used. In the case where an antioxidant is contained, the weight ratio of the antioxidant in the nonvolatile matter of the treating agent is not particularly limited, and is preferably from 0.1 to 5% by weight, preferably from 0.1 to 3% by weight.
此外,本發明的合成纖維用處理劑亦可以更含有原液穩定劑(例如,水、乙二醇、丙二醇)。原液穩定劑在處理劑中所佔的重量比率較佳為0.1至30重量%,更佳為1至20重量%。 Further, the treating agent for synthetic fibers of the present invention may further contain a stock solution stabilizer (for example, water, ethylene glycol, or propylene glycol). The weight ratio of the stock stabilizer to the treating agent is preferably from 0.1 to 30% by weight, more preferably from 1 to 20% by weight.
本發明的合成纖維用處理劑可以由僅包含不揮發成分的上述成分所構成,亦可以由不揮發成分與原液穩定劑所構成,也可為用低黏度礦物油稀釋過不揮發成分者,也可為將不揮發成分在水中乳化而成的水性乳液。在本發明的合成纖維用處理劑是將不揮發成分在水中乳化而成的水性乳液的情況下,不揮發成分的濃度較佳為5至35重量%,更佳為6至30重量%。從均勻賦予到纖維材料的觀點考慮,用低黏度礦物油稀釋不揮發成分後的處理劑的黏度(30℃)較佳為3至120mm2/s,更佳為5至100mm2/s。 The treatment agent for synthetic fibers of the present invention may be composed of the above-mentioned components containing only nonvolatile components, or may be composed of a nonvolatile component and a stock solution stabilizer, or may be a non-volatile component diluted with a low-viscosity mineral oil. It can be an aqueous emulsion obtained by emulsifying non-volatile components in water. In the case where the treating agent for synthetic fibers of the present invention is an aqueous emulsion obtained by emulsifying a nonvolatile component in water, the concentration of the nonvolatile component is preferably from 5 to 35% by weight, more preferably from 6 to 30% by weight. From the viewpoint of uniformly imparted to the fibrous material, the viscosity of the treatment agent is diluted with a low viscosity nonvolatile content of mineral oil (30 ℃) is preferably 3 to 120mm 2 / s, more preferably 5 to 100mm 2 / s.
本發明的合成纖維用處理劑的製造方法沒有特別限定,可以採用公知的方法。合成纖維用處理劑係藉由以任意或特定的順序將所構成的上述各成分添加混合而製造。從提高耐熱性的觀點考慮,各成分可以使用除去催化劑等並精製過者。特別是,本發明中使用的平滑成分(A)、非離子界面活性劑(D)中,會有含有無機物的情況,在使本發明的效果顯著降低的情況下,則除去無機物並進 行精製者為所期望的。作為除去無機物並進行精製的方法,能夠以公知的方法進行,例如,如果是平滑成分(A),則能夠藉由使用矽藻土的過濾從而除去,如果為非離子界面活性劑(D),則能夠藉由使用無機合成吸附劑的吸附除去從而進行精製。 The method for producing the treatment agent for synthetic fibers of the present invention is not particularly limited, and a known method can be employed. The treating agent for synthetic fibers is produced by adding and mixing the above-described respective components in an arbitrary or specific order. From the viewpoint of improving heat resistance, each component can be purified by removing a catalyst or the like. In particular, in the smoothing component (A) and the nonionic surfactant (D) used in the present invention, an inorganic substance may be contained, and when the effect of the present invention is remarkably lowered, the inorganic substance is removed. The line refiner is expected. The method of removing the inorganic substance and purifying it can be carried out by a known method. For example, if it is a smooth component (A), it can be removed by filtration using diatomaceous earth, and if it is a nonionic surfactant (D), The purification can be carried out by adsorption removal using an inorganic synthetic adsorbent.
本發明的合成纖維長絲紗線的製造方法係包括對原料合成纖維長絲紗線賦予本發明的合成纖維用處理劑。根據發明的製造方法,能夠降低浮渣或斷紗的產生,進而能夠得到紗品質優異的合成纖維長絲紗線。此外,本發明中的原料合成纖維長絲紗線是指未賦予處理劑的合成纖維長絲紗線。 The method for producing a synthetic fiber filament yarn of the present invention comprises applying a treating agent for a synthetic fiber of the present invention to a raw synthetic fiber filament yarn. According to the production method of the invention, it is possible to reduce the occurrence of scum or yarn breakage, and it is possible to obtain a synthetic fiber filament yarn excellent in yarn quality. Further, the raw material synthetic fiber filament yarn in the present invention means a synthetic fiber filament yarn to which no treating agent is imparted.
作為賦予合成纖維用處理劑的步驟,沒有特別限定,能夠採用公知的方法。通常係在原料合成纖維長絲紗線的紡紗步驟中賦予合成纖維用處理劑。在賦予處理劑之後,藉由熱輥進行拉伸、熱硬化(thermosetting)並卷取。如此,在具有賦予處理劑之後暫時不卷取而是進行熱拉伸的步驟的情況下,能夠適宜使用本發明的合成纖維用處理劑。作為熱拉伸時的溫度,可以列舉:在為聚酯、尼龍時,如果是工業物資用,則設想為210至260℃,如果是衣料用,則設想為110至220℃。 The step of imparting a treatment agent for synthetic fibers is not particularly limited, and a known method can be employed. The treating agent for synthetic fibers is usually imparted in the spinning step of the raw synthetic fiber filament yarn. After the treatment agent is applied, it is stretched by a heat roller, thermosetting, and wound up. In the case where the step of applying the treatment agent is not performed immediately after the application of the treatment agent, the treatment for synthetic fibers of the present invention can be suitably used. The temperature at the time of hot drawing is assumed to be 210 to 260 ° C in the case of polyester or nylon, and 110 to 220 ° C in the case of clothing.
賦予至原料合成纖維長絲紗線時的合成纖維處理劑如前所述,可以舉出:只包含不揮發成分的處理 劑、用低黏度礦物油稀釋不揮發成分過的處理劑、或者將不揮發成分在水中乳化後的水性乳液處理劑等。作為賦予方法,沒有特別限定,可以舉出:引導給油、輥給油、浸漬給油、噴霧給油等。其中,從賦予量的管理容易進行的點考慮,較佳引導給油、輥給油。 As described above, the synthetic fiber treating agent to be supplied to the raw material synthetic fiber filament yarn may be a treatment containing only a nonvolatile component. A treatment agent for diluting a non-volatile component with a low-viscosity mineral oil or an aqueous emulsion treatment agent for emulsifying a non-volatile component in water. The method of providing the method is not particularly limited, and examples thereof include a guide oil supply, a roll oil supply, a immersion oil supply, and a spray oil supply. Among them, it is preferable to guide the oil supply to the oil and the roller from the viewpoint of easy management of the amount of application.
相對於原料合成纖維長絲紗線,合成纖維用處理劑的不揮發成分的賦予量較佳為0.05至5重量%,更佳為0.1至3重量%,進一步更佳為0.1至2重量%。在小於0.05重量%時,會有無法發揮本發明的效果的情況。另一方面,在超過5重量%時,處理劑的不揮發成分容易脫落在紗道中,在熱輥上的焦油顯著增加,存在與絨毛、斷紗纏繞的情況。 The amount of the non-volatile component of the treating agent for synthetic fibers is preferably from 0.05 to 5% by weight, more preferably from 0.1 to 3% by weight, still more preferably from 0.1 to 2% by weight, based on the raw synthetic fiber filament yarn. When it is less than 0.05% by weight, the effect of the present invention may not be exhibited. On the other hand, when it exceeds 5% by weight, the nonvolatile matter of the treating agent is liable to fall off in the yarn path, and the tar on the heat roller is remarkably increased, and it may be entangled with the pile and the yarn.
作為(原料)合成纖維長絲紗線,可以舉出:聚酯纖維、聚醯胺纖維、聚烯烴纖維等合成纖維的長絲紗線。本發明的合成纖維用處理劑適用於聚酯纖維、聚醯胺纖維、聚烯烴纖維等合成纖維。作為聚酯纖維,可以舉出:以對苯二甲酸乙二酯為主要構成單元的聚酯(PET)、以三亞甲基對苯二甲酸乙二酯(trimethylene butylene ethyleneterephtalate)為主要構成單元的聚酯(PTT)、以伸丁基對苯二甲酸乙二酯(butylene ethyleneterephtalate)為主要結構單元的聚酯(PBT)、以乳酸為主要構成單元的聚酯(PLA)等,作為聚胺酯纖維,可以舉出:尼龍6、尼龍66等,作為聚烯烴纖維,可以舉出:聚丙烯、聚乙烯等。作為合成纖維長絲紗線的製造方法,沒有特別限定,能夠採用公知 的方法。 Examples of the (raw material) synthetic fiber filament yarn include a filament yarn of a synthetic fiber such as a polyester fiber, a polyamide fiber, or a polyolefin fiber. The treating agent for synthetic fibers of the present invention is suitable for use in synthetic fibers such as polyester fibers, polyamide fibers, and polyolefin fibers. Examples of the polyester fiber include polyester (PET) containing ethylene terephthalate as a main constituent unit and polytrimethylene butylene ethylene terephate (polymethylene butylene ethylene tereate) as a main constituent unit. Polyester (PTT), polyester (PBT) containing butylene ethylene terephthalate as main structural unit, and polyester (PLA) containing lactic acid as main component, as a polyurethane fiber, Examples thereof include nylon 6, nylon 66, and the like, and examples of the polyolefin fiber include polypropylene and polyethylene. The method for producing the synthetic fiber filament yarn is not particularly limited, and can be known. Methods.
本發明的纖維結構物係含有用上述的本發明的製造方法得到的合成纖維長絲紗線。具體而言,是使用已賦予本發明的合成纖維用處理劑的合成纖維長絲紗線,並利用噴水織機、噴氣織機或劍杆織機所織制成的織物以及利用圓形編織機、縱編織機或橫編織機所編制成的編物。此外,作為纖維結構物的用途,可以舉出:輪胎簾紗、安全帶、緩衝氣袋、漁網、繩索等工業材料、衣料用等。作為製造織物、編物的方法,沒有特別限定,能夠採用公知的方法。 The fiber structure of the present invention contains the synthetic fiber filament yarn obtained by the above-described production method of the present invention. Specifically, it is a synthetic fiber filament yarn to which the treating agent for synthetic fibers of the present invention has been applied, and is woven by a water jet loom, an air jet loom or a rapier loom, and a circular knitting machine or a longitudinal knitting machine. A braided machine or a knitting machine. Further, examples of the use of the fiber structure include industrial materials such as tire curtain yarns, safety belts, cushion air bags, fishing nets, and ropes, and clothing materials. The method for producing the woven fabric or the knitted fabric is not particularly limited, and a known method can be employed.
以下,藉由實施例說明本發明,本發明不限於在此記載的實施例。此外,文中及表中的“%”意味著“重量%”。 Hereinafter, the present invention will be described by way of examples, but the invention is not limited to the examples described herein. In addition, "%" in the text and in the table means "% by weight".
作為含有有機磺酸化合物(B)的原料X-1,係使用HOSTAPUR SAS93(Hoechst公司製造,有機磺酸化合物(B)93重量%)。在原料X-1中含有大量的芒硝。藉由離子色譜法對原料X-1中所包含的硫酸根離子(SO4 2-)及氯離子(Cl-)的含量(重量比率)進行測定,結果相對於有機磺酸化合物(B),硫酸根離子為25950ppm,氯離子為62ppm。 As the raw material X-1 containing the organic sulfonic acid compound (B), HOSTAPUR SAS93 (manufactured by Hoechst Co., Ltd., organic sulfonic acid compound (B): 93% by weight) was used. A large amount of thenardite is contained in the raw material X-1. The content (weight ratio) of the sulfate ion (SO 4 2- ) and the chloride ion (Cl - ) contained in the raw material X-1 is measured by ion chromatography, and as a result, relative to the organic sulfonic acid compound (B), The sulfate ion was 25,950 ppm and the chloride ion was 62 ppm.
作為含有有機磺酸化合物(B)的原料X-2,係使用Mersolat H95(拜耳公司製造,有機磺酸化合物(B))95重量%)。原料X-2中含有大量的氯化鈉。藉由離子色譜法對原料X-2中所包含的硫酸根離子(SO4 2-)及氯離子(Cl-)的含量(重量比率)進行測定,結果相對於有機磺酸化合物(B),硫酸根離子為820ppm,氯離子為30170ppm。 As the raw material X-2 containing the organic sulfonic acid compound (B), Mersolat H95 (manufactured by Bayer, organic sulfonic acid compound (B)) (5% by weight) was used. Raw material X-2 contains a large amount of sodium chloride. The content (weight ratio) of the sulfate ion (SO 4 2- ) and the chloride ion (Cl - ) contained in the raw material X-2 is measured by ion chromatography, and as a result, relative to the organic sulfonic acid compound (B), The sulfate ion was 820 ppm and the chloride ion was 30170 ppm.
含有有機磺酸化合物(B)的原料Y-1、Y-2係可以藉由對含有上述有機磺酸化合物(B)的原料X-1、X-2進行精製並除去無機物而得到。無機物的除去方法可以使用公知的方法,不限於實施例所示的精製方法。 The raw materials Y-1 and Y-2 containing the organic sulfonic acid compound (B) can be obtained by purifying the raw materials X-1 and X-2 containing the organic sulfonic acid compound (B) and removing the inorganic substances. A known method can be used for the method of removing the inorganic substance, and is not limited to the purification method shown in the examples.
將甲醇550份與離子交換水400份混合,以45±5℃進行調溫,在攪拌的同時緩緩投入700份的上述原料X-1,使其完全溶解。接著,將該溶解液在室溫下靜置20小時,使芒硝沉澱。取出不含芒硝的上清液,在60至80℃下進行減壓蒸餾,以除去甲醇與水的一部分,得到含有70重量%的有機磺酸化合物(B)的原料Y-1。 550 parts of methanol and 400 parts of ion-exchanged water were mixed, and the temperature was adjusted at 45 ± 5 ° C, and 700 parts of the above-mentioned raw material X-1 was gradually added while stirring to completely dissolve it. Next, the solution was allowed to stand at room temperature for 20 hours to precipitate Glauber's salt. The supernatant containing no Glauber's salt was taken out, and distilled under reduced pressure at 60 to 80 ° C to remove a part of methanol and water to obtain a raw material Y-1 containing 70% by weight of the organic sulfonic acid compound (B).
藉由離子色譜法對原料Y-1中所含的硫酸根離子(SO4 2-)及氯離子(Cl-)的含量(重量比率)進行測定,結果相對 於有機磺酸化合物(B),硫酸根離子為1085ppm,氯離子為60ppm。 The content (weight ratio) of the sulfate ion (SO 4 2- ) and the chloride ion (Cl - ) contained in the raw material Y-1 is measured by ion chromatography, and as a result, relative to the organic sulfonic acid compound (B), The sulfate ion was 1085 ppm and the chloride ion was 60 ppm.
將離子交換水600份加溫至80±5℃,並在攪拌的同時緩緩投入400份的上述原料X-2,使其完全溶解。接著,將該溶解液冷卻至40℃後,使用離子交換樹脂除去氯化鈉,得到含有40重量%的有機磺酸化合物(B)的原料Y-2。 600 parts of ion-exchanged water was heated to 80 ± 5 ° C, and 400 parts of the above-mentioned raw material X-2 was gradually added while stirring to completely dissolve it. Next, the solution was cooled to 40° C., and then sodium chloride was removed using an ion exchange resin to obtain a raw material Y-2 containing 40% by weight of the organic sulfonic acid compound (B).
藉由離子色譜法對原料Y-2所含有的硫酸根離子(SO4 2-)及氯離子(Cl-)的含量(重量比率)進行測定,結果相對於有機磺酸化合物(B),硫酸根離子為105ppm,氯離子為2115ppm。 The content (weight ratio) of the sulfate ion (SO 4 2- ) and the chloride ion (Cl - ) contained in the raw material Y-2 was measured by ion chromatography, and as a result, the sulfuric acid was compared with the organic sulfonic acid compound (B). The root ion was 105 ppm and the chloride ion was 2115 ppm.
於反應容器中加入異鯨蠟醇820份,在攪拌的同時在60±5℃下一邊注意反應溫度一邊以每次少量的方式投入五氧化二磷180份。然後,在75±5℃下熟成3小時,調製含有不揮發成分為100量%的有機磷酸酯化合物(C)的原料Z-1。 To the reaction vessel, 820 parts of iso-cetyl alcohol was added, and 180 parts of phosphorus pentoxide was introduced in a small amount at a temperature of 60 ± 5 ° C while stirring at 60 ± 5 ° C. Then, the mixture was aged at 75 ± 5 ° C for 3 hours to prepare a raw material Z-1 containing an organic phosphate compound (C) having a nonvolatile content of 100% by weight.
有機磷酸酯化合物(C1)、(C2)、(C3)、(C4)及無機磷酸的P核積分比率分別為33.05%、29.81%、33.82%、2.76%、0.56%。 The P core integration ratios of the organophosphate compounds (C1), (C2), (C3), (C4), and inorganic phosphoric acid were 33.05%, 29.81%, 33.82%, 2.76%, and 0.56%, respectively.
於反應器中加入C11至15的醇800份,在攪拌的同時在60±5℃下一邊注意反應溫度一邊以每次少量的方式投入五氧化二磷200份。然後,在75±5℃下熟成3小時,調製含有有機磷酸酯化合物(C)的原料Z-2。 To the reactor, 800 parts of an alcohol of C11 to 15 was added, and 200 parts of phosphorus pentoxide was introduced in a small amount while paying attention to the reaction temperature at 60 ± 5 ° C while stirring. Then, it was aged at 75 ± 5 ° C for 3 hours to prepare a raw material Z-2 containing the organic phosphate compound (C).
有機磷酸酯化合物(C1)、(C2)、(C3)、(C4)及無機磷酸的P核積分比率分別為44.23%、40.31%、13.79%、1.09%、0.58%。 The P core integration ratios of the organophosphate compounds (C1), (C2), (C3), (C4), and inorganic phosphoric acid were 44.23%, 40.31%, 13.79%, 1.09%, and 0.58%, respectively.
於上述調製的原料Z-2997份中投入離子交換水3份,在90℃下進行3小時的加水處理。然後,在115℃下進行3小時的脫水處理,調製含有有機磷酸酯化合物(C)的原料Z-3。 Three parts of ion-exchanged water was added to the raw material Z-2997 prepared above, and water addition treatment was performed at 90 ° C for 3 hours. Then, the mixture was subjected to a dehydration treatment at 115 ° C for 3 hours to prepare a raw material Z-3 containing the organic phosphate compound (C).
有機磷酸酯化合物(C1)、(C2)、(C3)、(C4)及無機磷酸的P核積分比率分別為56.72%、40.49%、0.00%、0.00%、2.78%。 The P core integration ratios of the organophosphate compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid were 56.72%, 40.49%, 0.00%, 0.00%, and 2.78%, respectively.
於反應容器中加入油醇600份,在攪拌的同時在70±5℃下一邊注意反應溫度一邊以每次少量的方式投入五氧化二磷110份。然後,在75±5℃下熟成3小時,調製含有有機磷酸酯化合物(C)的原料Z-4。 To the reaction vessel, 600 parts of oleyl alcohol was added, and 110 parts of phosphorus pentoxide was introduced in a small amount at a time of 70 ± 5 ° C while paying attention to the reaction temperature while stirring. Then, it was aged at 75 ± 5 ° C for 3 hours to prepare a raw material Z-4 containing the organic phosphate compound (C).
有機磷酸酯化合物(C1)、(C2)、(C3)、(C4)及無機磷酸 的P核積分比率分別為57.65%、35.26%、4.57%、0.44%、2.07%。 Organophosphate compounds (C1), (C2), (C3), (C4) and inorganic phosphates The P core integration ratios were 57.65%, 35.26%, 4.57%, 0.44%, and 2.07%, respectively.
於反應容器中加入油醇600份,在攪拌的同時在70±5℃下一邊注意反應溫度一邊以每次少量的方式投入五氧化二磷110份。然後,在70±5℃下熟成3小時。接著投入離子交換水15份,在90℃下進行3小時的加水處理,接著緩緩投入二丁基乙醇胺200份,以進行中和,調製含有有機磷酸酯化合物(C)的原料Z-5。 To the reaction vessel, 600 parts of oleyl alcohol was added, and 110 parts of phosphorus pentoxide was introduced in a small amount at a time of 70 ± 5 ° C while paying attention to the reaction temperature while stirring. Then, it was aged at 70 ± 5 ° C for 3 hours. Then, 15 parts of ion-exchanged water was added, and water addition treatment was performed at 90 ° C for 3 hours, and then 200 parts of dibutylethanolamine was gradually added to carry out neutralization to prepare a raw material Z-5 containing the organic phosphate compound (C).
有機磷酸酯化合物(C1)、(C2)、(C3)、(C4)及無機磷酸的P核積分比率分別為55.18%、35.38%、2.43%、0.00%、7.01%。 The P core integration ratios of the organophosphate compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid were 55.18%, 35.38%, 2.43%, 0.00%, and 7.01%, respectively.
於上述製備的970份的原料Z-1中投入離子交換水30份,在90℃下進行3小時的加水處理。然後,在115℃下進行3小時的脫水處理,調製含有有機磷酸酯化合物(C)的原料Z-3。 To 970 parts of the raw material Z-1 prepared above, 30 parts of ion-exchanged water was charged, and water treatment was performed at 90 ° C for 3 hours. Then, the mixture was subjected to a dehydration treatment at 115 ° C for 3 hours to prepare a raw material Z-3 containing the organic phosphate compound (C).
有機磷酸酯化合物(C1)、(C2)、(C3)、(C4)及無機磷酸的P核積分比率分別為65.43%、31.74%、0.00%、0.00%、2.83%。 The P core integration ratios of the organophosphate compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid were 65.43%, 31.74%, 0.00%, 0.00%, and 2.83%, respectively.
此外,有機磷酸酯化合物(C1)、(C2)、(C3)、(C4)及無機磷酸P核積分比率,係使用31P-NMR並藉由以 下方法算出。 Further, the organic phosphate compounds (C1), (C2), (C3), (C4) and the inorganic phosphate P core integral ratio were calculated by the following method using 31 P-NMR.
在直徑5mm的NMR用試驗管中稱量測定試樣的不揮發成分約30mg,加入約0.5ml的作為氘化溶劑之重水(D2O),使其溶解,使用31P-NMR測定裝置(BRUKER公司製造AVANCE400,162MHz)進行測定。 The non-volatile content of the measurement sample was weighed to about 30 mg in a test tube of NMR having a diameter of 5 mm, and about 0.5 ml of heavy water (D 2 O) as a deuterated solvent was added and dissolved, and a 31 P-NMR measuring device was used. BRUKER manufactures AVANCE 400, 162 MHz) for measurement.
將表2、3記載的成分混合,並攪拌至均勻為止,而調製處理劑。使用調製的各處理劑,以下述的方法評價針(pin)的污染累積、針的污染擦除性、張力變動。將其結果表示於表2、3。 The components described in Tables 2 and 3 were mixed and stirred until uniform, and a treatment agent was prepared. Using each of the prepared treatment agents, the contamination accumulation of the needle, the stain erasability of the needle, and the tension fluctuation were evaluated by the following methods. The results are shown in Tables 2 and 3.
此外,表2、3的處理劑的不揮發組成的數字係表示各成分(原料X、Y、Z為此等的不揮發成分)在處理劑的不揮發成分中所佔的重量比率。此外,表2、3的處理劑成分的詳細表示於表1。 Further, the numbers of the nonvolatile components of the treating agents in Tables 2 and 3 indicate the weight ratio of the respective components (nonvolatile components such as the raw materials X, Y, and Z) to the nonvolatile components of the treating agent. Further, the details of the treatment agent components of Tables 2 and 3 are shown in Table 1.
準確稱量試樣(處理劑的不揮發成分或原料X、Y、Z的不揮發成分)5g,在攪拌的同時以每次少量的方式加入超純水95g,製作水溶液,用100ml的容量瓶進行定容。將製作成的水溶液2ml通過ODS(使十八烷基與氧化矽凝膠化學鍵結後的)前處理管柱,將除去親油性物質後的液體供至離子色譜分析用。在以下的離子色譜分析條件下進行檢 測。利用對於已知濃度的標準液的譜峰面積比來測定檢測量,並換算硫酸根離子(SO4 2-)、磷酸根離子(PO4 3-)、氯離子(Cl-)的量。此外,定量極限係硫酸根離子(SO4 2-)為0.6ppm以下,氯離子(Cl-)為1.0ppm以下,磷酸根離子(PO4 3-)為0.3ppm以下。表2、3中的*表示定量極限以下。 Accurately weigh 5g of the sample (non-volatile component of the treatment agent or non-volatile components of the raw materials X, Y, Z), and add 95g of ultrapure water in a small amount each time while stirring to prepare an aqueous solution, using a 100ml volumetric flask. Make a constant volume. 2 ml of the prepared aqueous solution was passed through a pretreatment column of ODS (the octadecyl group was chemically bonded to the cerium oxide gel), and the liquid obtained by removing the lipophilic substance was supplied to ion chromatography. The detection was carried out under the following ion chromatography conditions. The amount of detection is determined by the peak area ratio of the standard solution of a known concentration, and the amounts of sulfate ion (SO 4 2- ), phosphate ion (PO 4 3- ), and chloride ion (Cl - ) are converted. Further, the quantitative limit is a sulfate ion (SO 4 2- ) of 0.6 ppm or less, a chloride ion (Cl - ) of 1.0 ppm or less, and a phosphate ion (PO 4 3- ) of 0.3 ppm or less. The * in Tables 2 and 3 indicates the quantitative limit or less.
<離子色譜條件> <Ion Chromatography Conditions>
裝置:Dionex製造ICS-1500使用抑制器 Device: Dionex manufactures ICS-1500 use suppressor
分析柱:Dionex IonPac AS14內徑4.0mm×長度50mm Analytical column: Dionex IonPac AS14 inner diameter 4.0mm × length 50mm
保護柱:Dionex IonPac AG14內徑4.0mm×長度250mm Guard column: Dionex IonPac AG14 inner diameter 4.0mm × length 250mm
洗脫液:3.5mmolNa2CO3、1.0mmolNaHCO3 Eluent: 3.5 mmol Na 2 CO 3 , 1.0 mmol NaHCO 3
流量:1.5ml/min Flow rate: 1.5ml/min
將上述製備的處理劑以定量20重量%的方式賦予至1000丹尼、96根的無給油聚酯長絲,使用掃紗法摩擦測定機使該長絲通過加熱至150℃的輥,除去揮發成分後,與加溫至250℃的緞紋鉻針接觸,並以初期張力500g、掃紗速度2m/分鐘移行4小時,評價針的污染累積程度、針的污染擦除性、張力變動。此外,為了進行更嚴密的評價,賦予20重量%的處理劑。 The treatment agent prepared above was applied to 1000 denier and 96 oil-free polyester filaments in a quantitative amount of 20% by weight, and the filament was passed through a roller heated to 150 ° C by a scuffing method to remove volatiles. After the composition, the mixture was brought into contact with a satin chrome needle heated to 250 ° C, and moved at an initial tension of 500 g and a sweep speed of 2 m/min for 4 hours to evaluate the degree of contamination accumulation of the needle, the stain erasability of the needle, and the tension fluctuation. Further, in order to carry out a more stringent evaluation, 20% by weight of a treating agent was imparted.
針的污染累積的程度通過下述基準進行評價。 The degree of contamination accumulation of the needle was evaluated by the following criteria.
◎:幾乎確認不到污染 ◎: almost no pollution is confirmed
○:稍微確認到污染 ○: A little confirmation of pollution
×:明顯有污染累積 ×: Significant pollution accumulation
張力變動值利用下式算出。 The tension variation value was calculated by the following formula.
張力變動值(g)=使紗移行4小時後的張力(g)-初期的張力(g) Tension variation value (g) = tension after moving the yarn for 4 hours (g) - initial tension (g)
此外,根據張力變動值利用下述基準評價張力變動。 Further, the tension fluctuation was evaluated based on the tension fluctuation value using the following criteria.
◎:0g至小於30g ◎: 0g to less than 30g
○:30g至小於50g ○: 30g to less than 50g
×:50g以上 ×: 50g or more
用下述方法評價針的污染擦除性。 The stain erasability of the needle was evaluated by the following method.
使將氫氧化鈉溶解於水與甘油中而成的溶液浸入紗布中,來擦除緞紋鉻針上產生的污染。以直到擦去所需要的次數,評價擦除性。 A solution obtained by dissolving sodium hydroxide in water and glycerin is immersed in the gauze to remove the contamination generated on the satin chrome needle. The erasability was evaluated by the number of times required until wiping off.
◎:以少於5次的擦除就能夠擦除污染 ◎: Can erase the pollution with less than 5 erases
○:以5次以上小於20次的擦除就能夠擦除污染 ○: Erasing can be erased by erasing 5 times or more and less than 20 times
×:以20次以上的擦除仍未擦除 ×: The erase is not erased after 20 or more erasures
從表2、3可知,實施例中,使用將從處理劑的不揮發成分中檢測出的硫酸根離子與氯離子設為規定比率以下的處理劑,因此幾乎沒有針的污染累積,擦除性極優異。亦即,能夠降低製造合成纖維時的輥污染,能夠增長輥的清掃間隔而減少其清掃次數。此外,張力變動值亦極小,能夠急劇減少絨毛、斷紗。 As is apparent from Tables 2 and 3, in the examples, the sulfate ion and the chloride ion detected from the nonvolatile component of the treatment agent are used as a treatment agent having a predetermined ratio or less. Therefore, there is almost no contamination accumulation of the needle, and the erasability is eliminated. Excellent. That is, it is possible to reduce roll contamination when manufacturing synthetic fibers, and it is possible to increase the cleaning interval of the rolls and reduce the number of times of cleaning. In addition, the tension variation value is also extremely small, and it is possible to drastically reduce fluff and yarn breakage.
另一方面,比較例中,從處理劑的不揮發成分中檢測出的硫酸根離子或氯離子的比率高,因此,針的污染累積多,擦除性不佳。此外,可知張力變動值極大,屢次產生絨毛、斷紗。 On the other hand, in the comparative example, since the ratio of the sulfate ion or the chloride ion detected from the nonvolatile component of the treatment agent is high, the contamination of the needle is excessively accumulated, and the erasability is poor. In addition, it can be seen that the value of the tension variation is extremely large, and the pile and the yarn are repeatedly generated.
本發明的合成纖維處理劑適合於防水帆布、輪胎簾紗、安全帶、氣囊、漁網、繩索、吊索等工業材料、織物或編物等衣料用等中所使用的合成纖維長絲紗線。 The synthetic fiber treating agent of the present invention is suitable for synthetic fiber filament yarns used in industrial materials such as waterproof canvas, tire curtain yarn, safety belt, airbag, fishing net, rope, sling, and the like for clothing and the like.
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TWI694194B (en) * | 2018-07-26 | 2020-05-21 | 日商竹本油脂股份有限公司 | Treatment agent for synthetic fiber and synthetic fiber |
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