CN108442115A - A kind of preparation method of spinning oil - Google Patents

A kind of preparation method of spinning oil Download PDF

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CN108442115A
CN108442115A CN201810137725.3A CN201810137725A CN108442115A CN 108442115 A CN108442115 A CN 108442115A CN 201810137725 A CN201810137725 A CN 201810137725A CN 108442115 A CN108442115 A CN 108442115A
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mass ratio
take
stirred
parts
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戴琪
张文文
杨颖�
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53—Polyethers
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/647—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/65—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy groups
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30—Flame or heat resistance, fire retardancy properties

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

Abstract

The invention discloses a kind of preparation methods of spinning oil, belong to field of textiles.The present invention is using long-chain alkyl tertiary amine as raw material, synthesis is with wetting, anlistatig characteristic, toxicity stimulates weak, degradable substance, it forms water suction conductive film in spinning process in fiber surface, reduce accumulation, improve its anlistatig performance, oriented attachment is easy to form interfacial film after fiber surface, interfacial film can absorb the moisture in air, and supply ion, and ion can move on this surface, therefore, energy is conductive and prevents static focus burnt, prevents and occurs coking on hot-rolling, to be easy to cause the phenomenon that lousiness is with breaking end.The problem of it is poor that the present invention solves current spinning oil antistatic property, is easy to focus, the poor heat resistance of product.

Description

A kind of preparation method of spinning oil
Technical field
The invention belongs to field of textiles, and in particular to a kind of preparation method of spinning oil.
Background technology
Spinning oil is synthetic fibers into fibre and weaves required auxiliary agent in process, can adjust fiber and fiber Between, friction coefficient between fiber and metal, reduce the electrostatic generated by friction, make fiber have good convergence, flatness and Fiber separation meets the needs of fiber post-processing concerned process steps.In spinning process, it is desirable to finish can quickly, uniformly in precursor table Face is sprawled, therefore it is required that finish has lower surface tension.Conventional surfactant such as fatty alcohol polyoxyethylene ether, fatty acid polyglycol Ethylene oxide ester etc..The main function of general filament yarn oil agent is that the fiber after oiling is enable successfully to be wound, silk cylinder forming, And lousiness, broken end are reduced in stretching process, ensure normal stretch, it requires that finish must also have good antistatic property With the wetability and fiber coherent, flatness, heat-resisting quantity of appropriateness.Recently as the high speed of spinning, the fine-denier of fiber Change, the development of functionalization and greenization, to oil performance, more stringent requirements are proposed.It is ground by the domestic preparation medium of years development Level processed has improved a lot, multiple serial tens kinds with independent intellectual property right, but also larger compared with external Gap, home brands spinning oil is still less than 25% in terms of occupation rate of market, and there is also the larger market demands.
Current spinning oil is mainly by wetting agent, collecting agent, smooth agent, emulsifier, antistatic agent and a small amount of softness The compositions such as agent, antifoaming agent.Although having certain effect, still antistatic property is poor, filametntary flatness is paid no attention to convergence Think.Domestic conventional spinning finish is using single phosphate or to be equipped with using β-alkylsulfonate as antistatic agent, wet Spend it is lower in the case of, antistatic property substantially reduces, using this fibre finishing just by great limitation, and product Poor heat resistance, once exceeding 130 DEG C, spinning oil just volatilizees seriously the heating roller temperature when continuous production, is easy to make in workshop Larger smog is generated, causes the working environment of workers poor, while seriously affecting the health of worker.Therefore, it produces a kind of anti- The good and heat-resisting spinning oil of antistatic property has the prodigious market demand.
Invention content
The technical problems to be solved by the invention：It is poor for current spinning oil antistatic property, it is easy to focus, product The problem of poor heat resistance, provides a kind of preparation method of spinning oil.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of spinning oil, which is characterized in that the preparation method includes the following steps：
（1）Take hexadecyldimethyl benzyl ammonium tertiary amine in mass ratio 1：2：10 are added chlorethanol, the ethanol solution that mass fraction is 80% mixes It closes, stirs 20 ~ 30min, add the sodium carbonate of chlorethanol quality 0.2 ~ 0.5%, be stirred at reflux 5 ~ 6h of holding, be evaporated under reduced pressure, obtain It is evaporated under reduced pressure object A, takes vacuum distillation object A by quality 1：3 are added epoxychloropropane, adjust pH to 8 ~ 9, are stirred, must stir Mixture A；
（2）Take stirring mixture A in mass ratio 1：9 are added absolute ethyl alcohol mixing, and 30 ~ 50min, filtering is kept to take filtrate A by matter Measure ratio 1：5 are added acetone, stand, obtain standing liquid, take and stand liquid in mass ratio 1：2 are added polyethylene glycol mixing, obtain mixture, press Mass fraction meter takes 6 ~ 9 parts of mixtures, 60 ~ 80 parts of acetone, 1 ~ 2 part of boron trifluoride ether, is stirred 2 ~ 4h, vacuum distillation, Object B must be evaporated under reduced pressure；
（3）Take vacuum distillation object B in mass ratio 3：6~9：2 are added carbon tetrachloride, phosphorus pentoxide mixing, are stirred to react, must stir Reactant is mixed, reaction stirred in mass ratio 10 is taken：1, which is added the potassium hydroxide that mass fraction is 30%, mixes, and obtains mixed liquor, takes Mixed liquor in mass ratio 2：7 are added ether extraction, and rotary evaporation is evaporated under reduced pressure, and concentration obtains concentrate；
（4）Take oxidized polyethylene wax in mass ratio 1：10 addition deionized waters are stirred, and mixture B must be stirred, by mass parts Number meter takes 20 ~ 30 parts of stirring mixture B, 6 ~ 8 parts of peregal os-15s, 0.05 ~ 0.1 part of polyethylene glycol mixing, it is warming up to 120 ~ 130 DEG C, 40r/min 60 ~ 70min of holding, are cooled to room temperature, obtain cooling thing, according to the mass fraction, take 1 ~ 2 part of lauric acid polyoxy Vinyl acetate, 6 ~ 8 parts of Polyethylene Glycol Oleates, 20 ~ 30 parts of concentrates, 10 ~ 15 parts of cooling thing mixing, keep 1 ~ 2h, obtain spinning oil Agent matrix object, it is spare；
（5）Allyl polyether is taken in 65 ~ 70 DEG C of 20 ~ 30min of vacuum outgas, is passed through nitrogen, be added allyl polyether quality 0.5 ~ The epoxychloropropane of 0.7% stannous chloride and allyl polyether quality 40 ~ 50%, in 65 ~ 70 DEG C keep 2 ~ 3h, rotary evaporation, Rotary evaporation object A is obtained, rotary evaporation object A in mass ratio 1 is taken：8：2 are added toluene, mass fraction as 30% sodium hydroxide solution Mixing keeps 1 ~ 2h, filtering to take liquor B, adjusts pH to 7 ~ 7.2, rotary evaporation is dry, obtains dried object；
（6）Take dried object in mass ratio 800 ~ 900：3~4：1 ~ 2 is added chloroplatinic acid, isopropanol, is passed through nitrogen, and stir-activating 1 ~ 2h adds the 1 of dried object quality 20 ~ 30%, 1,3,3- tetramethyl and siloxanes, is stirred to react, obtains reactive matrix object, takes eight Methyl cyclotetrasiloxane in mass ratio 9：2 are added tetramethylammonium hydroxide mixing, keep 30 ~ 40min in 60 ~ 65 DEG C, add The reactive matrix object of 2 ~ 3 times of octamethylcy-clotetrasiloxane keeps 3 ~ 4h, rotary evaporation to obtain rotary evaporation object B, take rotary evaporation Object B in mass ratio 2：4 ~ 5 are added step（4）Spare spinning oil matrix object mixes to get spinning oil.
Compared with other methods, advantageous effects are the present invention：
（1）Using long-chain alkyl tertiary amine as raw material, synthesis stimulates weak, degradable the present invention with wetting, anlistatig characteristic, toxicity Substance, in spinning process fiber surface formed water suction conductive film, reduce accumulation, improve its anlistatig property Can, oriented attachment is easy to form interfacial film after fiber surface, and interfacial film can absorb the moisture in air, and supply ion, from Son can move on this surface, and therefore, energy is conductive and prevents static focus burnt, prevents and occurs coking on hot-rolling, to be easy The phenomenon that causing lousiness and broken end；
（2）The present invention is polyethylene wax under oxidant effect, and oxidation reaction occurs under appropriate circumstances and generates, gained Microemulsion have that good filming performance, fusing point be high, good toughness, add and contain long carbon in emulsifier peregal os-15 molecule Chain hydrophobic grouping only introduces some polar groups after oxidation in long alkane structure, and progress that can be better is newborn Change, be added dispersant polyethylene glycol, it can be made to be uniformly dispersed in aqueous emulsion, in high temperature spinning process with fiber It crosslinks, generates long branched structure and be attached to fiber surface, plasticization is played to fiber, prevent fiber anti-with finishing agent It answers degree excessively high, reduces even reinforcing fiber loss, improve fiber flexibility, improve filametntary Lubricity, simultaneously The elasticity for increasing strand makes crosslinked fiber have preferable relaxation energy by the movement of strand under stress Power, the tensile strength of the fiber also improved；
（3）The present invention synthesizes a kind of polyepoxide-polyether using hydrosilylation using allyl polyether, epoxychloropropane as raw material The heat resistance of product can be improved using epoxy group for modified silicon oil, and the hydrophily of product can be improved in polyether group, and stability is good, It sprawls film forming in filament surfaces at high temperature, and the coefficient of conductivity is low, effectively delays heat and is passed to inside precursor, while It delays since the small molecule that precursor thermal decomposition generates is discharged into the external time, there is good heat resistance.
Specific implementation mode
Lauric acid polyoxyethylene ester, Polyethylene Glycol Oleate, allyl polyether：It is purchased from Jiangsu Hai'an petrochemical plant.
A kind of preparation method of spinning oil, includes the following steps：
（1）Take hexadecyldimethyl benzyl ammonium tertiary amine in mass ratio 1：2：10 are added chlorethanol, the ethanol solution that mass fraction is 80% mixes It closes, stirs 20 ~ 30min, add the sodium carbonate of chlorethanol quality 0.2 ~ 0.5%, 80 ~ 85 DEG C are stirred at reflux 5 ~ 6h of holding, decompression Distillation, must be evaporated under reduced pressure object A, take vacuum distillation object A by quality 1：3 are added epoxychloropropane, adjust pH to 8 ~ 9, are stirred 2 ~ 3h must stir mixture A；
（2）Take stirring mixture A in mass ratio 1：9 are added absolute ethyl alcohol mixing, and 30 ~ 50min, filtering is kept to take filtrate A by matter Measure ratio 1：5 are added acetone, stand 3 ~ 4h, obtain standing liquid, take and stand liquid in mass ratio 1：2 be added polyethylene glycol mixing 15 ~ 20min obtains mixture, according to the mass fraction, takes 6 ~ 9 parts of mixtures, 60 ~ 80 parts of acetone, 1 ~ 2 part of boron trifluoride ether, stirring 2 ~ 4h is mixed, vacuum distillation must be evaporated under reduced pressure object B；
（3）Take vacuum distillation object B in mass ratio 3：6~9：2 are added carbon tetrachloride, phosphorus pentoxide mixing, are stirred to react 2 ~ 4h, Reaction stirred is obtained, reaction stirred in mass ratio 10 is taken：1, which is added the potassium hydroxide that mass fraction is 30%, mixes, and must mix Liquid takes mixed liquor in mass ratio 2：7 are added ether extraction, and rotary evaporation is evaporated under reduced pressure, and concentration obtains concentrate；
（4）Take oxidized polyethylene wax in mass ratio 1：10 addition deionized waters are stirred, and mixture B must be stirred, by mass parts Number meter takes 20 ~ 30 parts of stirring mixture B, 6 ~ 8 parts of peregal os-15s, 0.05 ~ 0.1 part of polyethylene glycol mixing, it is warming up to 120 ~ 130 DEG C, 40r/min 60 ~ 70min of holding, are cooled to room temperature, obtain cooling thing, according to the mass fraction, take 1 ~ 2 part of lauric acid polyoxy Vinyl acetate, 6 ~ 8 parts of Polyethylene Glycol Oleates, 20 ~ 30 parts of concentrates, 10 ~ 15 parts of cooling thing mixing, keep 1 ~ 2h, obtain spinning oil Agent matrix object, it is spare；
（5）Allyl polyether is taken in 65 ~ 70 DEG C of 20 ~ 30min of vacuum outgas, is passed through nitrogen, be added allyl polyether quality 0.5 ~ The epoxychloropropane of 0.7% stannous chloride and allyl polyether quality 40 ~ 50%, in 65 ~ 70 DEG C keep 2 ~ 3h, rotary evaporation, Rotary evaporation object A is obtained, rotary evaporation object A in mass ratio 1 is taken：8：2 are added toluene, mass fraction as 30% sodium hydroxide solution Mixing keeps 1 ~ 2h, filtering to take liquor B, adjusts pH to 7 ~ 7.2, rotary evaporation is dry, obtains dried object；
（6）Take dried object in mass ratio 800 ~ 900：3~4：1 ~ 2 is added chloroplatinic acid, isopropanol, is passed through nitrogen, and stir-activating 1 ~ 2h adds the 1 of dried object quality 20 ~ 30%, 1,3,3- tetramethyl and siloxanes, is stirred to react 3 ~ 4h, obtains reactive matrix object, Take octamethylcy-clotetrasiloxane in mass ratio 9：2 are added tetramethylammonium hydroxide mixing, and 30 ~ 40min is kept in 60 ~ 65 DEG C, then The reactive matrix object of 2 ~ 3 times of octamethylcy-clotetrasiloxane is added, 3 ~ 4h, rotary evaporation is kept to obtain rotary evaporation object B, take rotation Evaporant B in mass ratio 2：4 ~ 5 are added step（4）Spare spinning oil matrix object mixes to get spinning oil.
Embodiment 1
Lauric acid polyoxyethylene ester, Polyethylene Glycol Oleate, allyl polyether：It is purchased from Jiangsu Hai'an petrochemical plant.
A kind of preparation method of spinning oil, includes the following steps：
（1）Take hexadecyldimethyl benzyl ammonium tertiary amine in mass ratio 1：2：10 are added chlorethanol, the ethanol solution that mass fraction is 80% mixes It closes, stirs 20min, add the sodium carbonate of chlorethanol quality 0.2%, 80 DEG C are stirred at reflux holding 5h, and vacuum distillation must depressurize Distillation A takes vacuum distillation object A by quality 1：3 are added epoxychloropropane, adjust pH to 8, are stirred 2h, must be stirred Object A；
（2）Take stirring mixture A in mass ratio 1：9 are added absolute ethyl alcohol mixing, and 30min, filtering is kept to take filtrate A by quality Than 1：5 are added acetone, stand 3h, obtain standing liquid, take and stand liquid in mass ratio 1：2 are added polyethylene glycol mixing 15min, must mix Object takes 6 parts of mixtures, 60 parts of acetone, 1 part of boron trifluoride ether, is stirred 2h according to the mass fraction, and vacuum distillation must subtract Press distillation B；
（3）Take vacuum distillation object B in mass ratio 3：6：2 are added carbon tetrachloride, phosphorus pentoxide mixing, are stirred to react 2h, must stir Reactant is mixed, reaction stirred in mass ratio 10 is taken：1, which is added the potassium hydroxide that mass fraction is 30%, mixes, and obtains mixed liquor, takes Mixed liquor in mass ratio 2：7 are added ether extraction, and rotary evaporation is evaporated under reduced pressure, and concentration obtains concentrate；
（4）Take oxidized polyethylene wax in mass ratio 1：10 addition deionized waters are stirred, and mixture B must be stirred, by mass parts Number meter takes 20 parts of stirring mixture B, 6 parts of peregal os-15s, 0.05 part of polyethylene glycol mixing, is warming up to 120 DEG C, 40r/min 60min is kept, is cooled to room temperature, obtains cooling thing, according to the mass fraction, take 1 part of lauric acid polyoxyethylene ester, 6 parts of poly- second of oleic acid Diol ester, 20 parts of concentrates, 10 parts of cooling thing mixing, keep 1h, obtain spinning oil matrix object, spare；
（5）It takes allyl polyether in 65 DEG C of vacuum outgas 20min, is passed through nitrogen, the chlorination of allyl polyether quality 0.5% is added The epoxychloropropane of stannous and allyl polyether quality 40% keeps 2h, rotary evaporation to obtain rotary evaporation object A, take rotation in 65 DEG C Turn evaporant A in mass ratio 1：8：2 are added toluene, the sodium hydroxide solution that mass fraction is 30% mixes, and 1h, filtering is kept to take Liquor B adjusts pH to 7, and rotary evaporation is dry, obtains dried object；
（6）Take dried object in mass ratio 800：3：1 is added chloroplatinic acid, isopropanol, is passed through nitrogen, stir-activating 1h is added dry The 1 of dry amount of substance 20%, 1,3,3- tetramethyl and siloxanes are stirred to react 3h, obtain reactive matrix object, take four silica of prestox ring Alkane in mass ratio 9：2 are added tetramethylammonium hydroxide mixing, keep 30min in 60 DEG C, add 2 times of octamethylcy-clotetrasiloxane Reactive matrix object, keep 3h, rotary evaporation obtains rotary evaporation object B, take rotary evaporation object B in mass ratio 2：4 are added step （4）Spare spinning oil matrix object mixes to get spinning oil.
Embodiment 2
Lauric acid polyoxyethylene ester, Polyethylene Glycol Oleate, allyl polyether：It is purchased from Jiangsu Hai'an petrochemical plant.
A kind of preparation method of spinning oil, includes the following steps：
（1）Take hexadecyldimethyl benzyl ammonium tertiary amine in mass ratio 1：2：10 are added chlorethanol, the ethanol solution that mass fraction is 80% mixes It closes, stirs 30min, add the sodium carbonate of chlorethanol quality 0.5%, 85 DEG C are stirred at reflux holding 6h, and vacuum distillation must depressurize Distillation A takes vacuum distillation object A by quality 1：3 are added epoxychloropropane, adjust pH to 9, are stirred 3h, must be stirred Object A；
（2）Take stirring mixture A in mass ratio 1：9 are added absolute ethyl alcohol mixing, and 50min, filtering is kept to take filtrate A by quality Than 1：5 are added acetone, stand 4h, obtain standing liquid, take and stand liquid in mass ratio 1：2 are added polyethylene glycol mixing 20min, must mix Object takes 9 parts of mixtures, 80 parts of acetone, 2 parts of boron trifluoride ether, is stirred 4h according to the mass fraction, and vacuum distillation must subtract Press distillation B；
（3）Take vacuum distillation object B in mass ratio 3：9：2 are added carbon tetrachloride, phosphorus pentoxide mixing, are stirred to react 4h, must stir Reactant is mixed, reaction stirred in mass ratio 10 is taken：1, which is added the potassium hydroxide that mass fraction is 30%, mixes, and obtains mixed liquor, takes Mixed liquor in mass ratio 2：7 are added ether extraction, and rotary evaporation is evaporated under reduced pressure, and concentration obtains concentrate；
（4）Take oxidized polyethylene wax in mass ratio 1：10 addition deionized waters are stirred, and mixture B must be stirred, by mass parts Number meter takes 30 parts of stirring mixture B, 8 parts of peregal os-15s, 0.1 part of polyethylene glycol mixing, is warming up to 130 DEG C, 40r/min guarantors 70min is held, is cooled to room temperature, cooling thing is obtained, according to the mass fraction, takes the poly- second of 2 parts of lauric acid polyoxyethylene esters, 8 parts of oleic acid two Alcohol ester, 30 parts of concentrates, 15 parts of cooling thing mixing, keep 2h, obtain spinning oil matrix object, spare；
（5）It takes allyl polyether in 70 DEG C of vacuum outgas 30min, is passed through nitrogen, the chlorination of allyl polyether quality 0.7% is added The epoxychloropropane of stannous and allyl polyether quality 50% keeps 3h, rotary evaporation to obtain rotary evaporation object A, take rotation in 70 DEG C Turn evaporant A in mass ratio 1：8：2 are added toluene, the sodium hydroxide solution that mass fraction is 30% mixes, and 2h, filtering is kept to take Liquor B adjusts pH to 7.2, and rotary evaporation is dry, obtains dried object；
（6）Take dried object in mass ratio 900：4：2 are added chloroplatinic acid, isopropanol, are passed through nitrogen, stir-activating 2h is added dry The 1 of dry amount of substance 30%, 1,3,3- tetramethyl and siloxanes are stirred to react 4h, obtain reactive matrix object, take four silica of prestox ring Alkane in mass ratio 9：2 are added tetramethylammonium hydroxide mixing, keep 40min in 65 DEG C, add 3 times of octamethylcy-clotetrasiloxane Reactive matrix object, keep 4h, rotary evaporation obtains rotary evaporation object B, take rotary evaporation object B in mass ratio 2：5 are added step （4）Spare spinning oil matrix object mixes to get spinning oil.
Embodiment 3
Lauric acid polyoxyethylene ester, Polyethylene Glycol Oleate, allyl polyether：It is purchased from Jiangsu Hai'an petrochemical plant.
A kind of preparation method of spinning oil, includes the following steps：
（1）Take hexadecyldimethyl benzyl ammonium tertiary amine in mass ratio 1：2：10 are added chlorethanol, the ethanol solution that mass fraction is 80% mixes It closes, stirs 25min, add the sodium carbonate of chlorethanol quality 0.35%, 83 DEG C are stirred at reflux holding 5.5h, and vacuum distillation must subtract Distillation A is pressed, takes vacuum distillation object A by quality 1：3 are added epoxychloropropane, adjust pH to 8.5, are stirred 2.5h, must stir Mix mixture A；
（2）Take stirring mixture A in mass ratio 1：9 are added absolute ethyl alcohol mixing, and 40min, filtering is kept to take filtrate A by quality Than 1：5 are added acetone, stand 3.5h, obtain standing liquid, take and stand liquid in mass ratio 1：2 are added polyethylene glycol mixing 17.5min, obtain Mixture takes 7.5 parts of mixtures, 70 parts of acetone, 1.5 parts of boron trifluoride ether, is stirred 3h according to the mass fraction, decompression Distillation, must be evaporated under reduced pressure object B；
（3）Take vacuum distillation object B in mass ratio 3：7.5：2 are added carbon tetrachloride, phosphorus pentoxide mixing, are stirred to react 3h, obtain Reaction stirred takes reaction stirred in mass ratio 10：1, which is added the potassium hydroxide that mass fraction is 30%, mixes, and obtains mixed liquor, Take mixed liquor in mass ratio 2：7 are added ether extraction, and rotary evaporation is evaporated under reduced pressure, and concentration obtains concentrate；
（4）Take oxidized polyethylene wax in mass ratio 1：10 addition deionized waters are stirred, and mixture B must be stirred, by mass parts Number meter takes 25 parts of stirring mixture B, 7 parts of peregal os-15s, 0.075 part of polyethylene glycol mixing, is warming up to 125 DEG C, 40r/ Min keeps 65min, is cooled to room temperature, obtains cooling thing, according to the mass fraction, takes 1.5 parts of lauric acid polyoxyethylene esters, 7 parts of oleic acid Macrogol ester, 25 parts of concentrates, 12.5 parts of cooling thing mixing, keep 1.5h, obtain spinning oil matrix object, spare；
（5）It takes allyl polyether in 67 DEG C of vacuum outgas 25min, is passed through nitrogen, the chlorination of allyl polyether quality 0.6% is added The epoxychloropropane of stannous and allyl polyether quality 45% keeps 2.5h, rotary evaporation to obtain rotary evaporation object A, take in 67 DEG C Rotary evaporation object A in mass ratio 1：8：2 are added toluene, the sodium hydroxide solution that mass fraction is 30% mixes, and keep 1.5h, mistake Filter takes liquor B, adjusts pH to 7.1, rotary evaporation is dry, obtains dried object；
（6）Take dried object in mass ratio 850：3.5：1.5 are added chloroplatinic acids, isopropanol, are passed through nitrogen, stir-activating 1.5h, then It is added 1,1,3,3- tetramethyl of dried object quality 25% and siloxanes, is stirred to react 3.5h, obtains reactive matrix object, take prestox Cyclotetrasiloxane in mass ratio 9：2 are added tetramethylammonium hydroxide mixing, keep 35min in 63 DEG C, add prestox ring four The reactive matrix object of 2.5 times of siloxanes keeps 3.5h, rotary evaporation to obtain rotary evaporation object B, take rotary evaporation object B in mass ratio 2：4.5 are added step（4）Spare spinning oil matrix object mixes to get spinning oil.
Comparative example：The spinning oil of Hangzhou company production.
The present invention is relatively shown in Table 1 with each application performance of spinning oil that comparative example uses.Spinning oil is in similarity condition It is 4500m/min that 15 day time, spinning speed are used in 16 spinning positions, and fiber dimensious 150D/96F, GR2 temperature is 130 ℃。
Table 1：
In summary, product of the invention temperature of smoldering will be higher by commercial product, and heat resistance advantage is significantly embodied.From From the point of view of antistatic property effect, it is better than other products performance, product comprehensive performance of the invention is better than presently commercially available product, is worth It promotes.

Claims (1)

1. a kind of preparation method of spinning oil, which is characterized in that the preparation method includes the following steps：
（1）Take hexadecyldimethyl benzyl ammonium tertiary amine in mass ratio 1：2：10 are added chlorethanol, the ethanol solution that mass fraction is 80% mixes It closes, stirs 20 ~ 30min, add the sodium carbonate of chlorethanol quality 0.2 ~ 0.5%, be stirred at reflux 5 ~ 6h of holding, be evaporated under reduced pressure, obtain It is evaporated under reduced pressure object A, takes vacuum distillation object A by quality 1：3 are added epoxychloropropane, adjust pH to 8 ~ 9, are stirred, must stir Mixture A；
（2）Take stirring mixture A in mass ratio 1：9 are added absolute ethyl alcohol mixing, and 30 ~ 50min, filtering is kept to take filtrate A by matter Measure ratio 1：5 are added acetone, stand, obtain standing liquid, take and stand liquid in mass ratio 1：2 are added polyethylene glycol mixing, obtain mixture, press Mass fraction meter takes 6 ~ 9 parts of mixtures, 60 ~ 80 parts of acetone, 1 ~ 2 part of boron trifluoride ether, is stirred 2 ~ 4h, vacuum distillation, Object B must be evaporated under reduced pressure；
（3）Take vacuum distillation object B in mass ratio 3：6~9：2 are added carbon tetrachloride, phosphorus pentoxide mixing, are stirred to react, must stir Reactant is mixed, reaction stirred in mass ratio 10 is taken：1, which is added the potassium hydroxide that mass fraction is 30%, mixes, and obtains mixed liquor, takes Mixed liquor in mass ratio 2：7 are added ether extraction, and rotary evaporation is evaporated under reduced pressure, and concentration obtains concentrate；
（4）Take oxidized polyethylene wax in mass ratio 1：10 addition deionized waters are stirred, and mixture B must be stirred, by mass parts Number meter takes 20 ~ 30 parts of stirring mixture B, 6 ~ 8 parts of peregal os-15s, 0.05 ~ 0.1 part of polyethylene glycol mixing, it is warming up to 120 ~ 130 DEG C, 40r/min 60 ~ 70min of holding, are cooled to room temperature, obtain cooling thing, according to the mass fraction, take 1 ~ 2 part of lauric acid polyoxy Vinyl acetate, 6 ~ 8 parts of Polyethylene Glycol Oleates, 20 ~ 30 parts of concentrates, 10 ~ 15 parts of cooling thing mixing, keep 1 ~ 2h, obtain spinning oil Agent matrix object, it is spare；
（5）Allyl polyether is taken in 65 ~ 70 DEG C of 20 ~ 30min of vacuum outgas, is passed through nitrogen, be added allyl polyether quality 0.5 ~ The epoxychloropropane of 0.7% stannous chloride and allyl polyether quality 40 ~ 50%, in 65 ~ 70 DEG C keep 2 ~ 3h, rotary evaporation, Rotary evaporation object A is obtained, rotary evaporation object A in mass ratio 1 is taken：8：2 are added toluene, mass fraction as 30% sodium hydroxide solution Mixing keeps 1 ~ 2h, filtering to take liquor B, adjusts pH to 7 ~ 7.2, rotary evaporation is dry, obtains dried object；
（6）Take dried object in mass ratio 800 ~ 900：3~4：1 ~ 2 is added chloroplatinic acid, isopropanol, is passed through nitrogen, and stir-activating 1 ~ 2h adds the 1 of dried object quality 20 ~ 30%, 1,3,3- tetramethyl and siloxanes, is stirred to react, obtains reactive matrix object, takes eight Methyl cyclotetrasiloxane in mass ratio 9：2 are added tetramethylammonium hydroxide mixing, keep 30 ~ 40min in 60 ~ 65 DEG C, add The reactive matrix object of 2 ~ 3 times of octamethylcy-clotetrasiloxane keeps 3 ~ 4h, rotary evaporation to obtain rotary evaporation object B, take rotary evaporation Object B in mass ratio 2：4 ~ 5 are added step（4）Spare spinning oil matrix object mixes to get spinning oil.
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Publication number Priority date Publication date Assignee Title
CN1143988A (en) * 1994-01-14 1997-02-26 丹拿克朗有限公司 Cardable hydrophobic polyolefin fibres comprising cationic spin finishes
CN101235592A (en) * 2008-03-07 2008-08-06 吴江市良燕纺织助剂厂 Terylene FDY nano spinning oil and preparation method thereof
CN102505482A (en) * 2011-11-02 2012-06-20 上虞市皇马化学有限公司 Novel chinlon cord thread oil agent and preparation method thereof
CN102619090A (en) * 2011-01-27 2012-08-01 上海雅运纺织助剂有限公司 Smoothening softener composition for cotton and its blended yarns, and preparation method thereof
CN105297427A (en) * 2015-10-23 2016-02-03 威海新元化工有限公司 Compound for improving heat resistance of amino-modified silicone oil carbon fiber oil formulation and preparation and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1143988A (en) * 1994-01-14 1997-02-26 丹拿克朗有限公司 Cardable hydrophobic polyolefin fibres comprising cationic spin finishes
CN101235592A (en) * 2008-03-07 2008-08-06 吴江市良燕纺织助剂厂 Terylene FDY nano spinning oil and preparation method thereof
CN102619090A (en) * 2011-01-27 2012-08-01 上海雅运纺织助剂有限公司 Smoothening softener composition for cotton and its blended yarns, and preparation method thereof
CN102505482A (en) * 2011-11-02 2012-06-20 上虞市皇马化学有限公司 Novel chinlon cord thread oil agent and preparation method thereof
CN105297427A (en) * 2015-10-23 2016-02-03 威海新元化工有限公司 Compound for improving heat resistance of amino-modified silicone oil carbon fiber oil formulation and preparation and application thereof

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Application publication date: 20180824