CN109763326A - A kind of anti-oxidant Antistatic spinning finish - Google Patents
A kind of anti-oxidant Antistatic spinning finish Download PDFInfo
- Publication number
- CN109763326A CN109763326A CN201910028968.8A CN201910028968A CN109763326A CN 109763326 A CN109763326 A CN 109763326A CN 201910028968 A CN201910028968 A CN 201910028968A CN 109763326 A CN109763326 A CN 109763326A
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- spinning
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a kind of anti-oxidant Antistatic spinning finishs, belong to synthetic fibers auxiliary agent technical field.One aspect of the present invention introduces silicon and the dual ignition-proof element of phosphorus in spinning oil, forms fire-resisting protection to fiber surface after oiling to spinning oil, on the other hand carries out phosphorylation reaction using phosphorus trichloride and ether compound, so that antistatic effect improves.The heat resistance that introducing propylene oxide chain link improves spinning oil is good, so that the coking phenomenon in spinning surface is greatly lowered, to improve the lousiness of fiber, fracture of wire phenomenon.It is arranged by the chain link of pfpe molecule chain, forms continuous oil film and carry out spinning protection.Using the amido bond of introducing, there is preferable polarity and stability, it is using the branched structure of skeleton structure that antioxidant is evenly dispersed in finish, improve spinning oil performance.The present invention solves the antistatic property difference of current spinning oil and winding, breakage phenomena occurs, finish is easy to oxidize and the problem of cause fabric easily to turn yellow.
Description
Technical field
The invention belongs to synthetic fibers auxiliary agent technical fields, and in particular to a kind of anti-oxidant Antistatic spinning finish.
Background technique
The adhesiveness that synthetic fibers do not have surface of natural fibers special, therefore during fibre spinning, preparation medium
Using essential.By using the frictional behavior of the adjustable fiber of finish, accumulation of static electricity is prevented or eliminated, control between tow
Cohesive force, assign the good convergence of fiber, flatness and fiber separation, it is ensured that synthetic fiber spinning is gone on smoothly.Fiber surface
Finish contacted first with production equipment, under conditions of raw material and production process equipment determine, the configuration of finish is to being produced into
Originally, production efficiency and product quality all have a significant impact.Existing chemical fibre is with finish mainly by smooth agent, collecting agent, antistatic
The composition such as agent, emulsifier and equilibrium modifier；But due to the difference of its constituent component, easily occur in spinning process lousiness,
Phenomena such as broken end, lead to that coiling and molding is poor, excellence rate is low, corrosion phenomenon is serious, it is difficult to adapt to the demand of spinning technique.
During experimental branch line and post-processing, in order to there is preferable spinnability, it is necessary to eliminate the electrostatic of precursor, adjustment rubs
Coefficient is wiped, fiber is assigned smoothly and flexibility, fiber is made to pass through the works such as spinning, drawing-off, winding, twisting, winder, weaving
Sequence, it is therefore necessary to spinning oil appropriate be added.The component of common preparation medium can be divided into two major classes: first major class packet
Including group composition is smooth agent, antistatic agent, emulsifier, and the second major class is accessory constituent, including wetting agent, softening agent, obvolvent agent, anti-
Oxidant, point fine agent, bleeding agent, pH adjusting agent, viscosity-improving agents, stabilizer, defoaming agent, antimicrobial, preservative and
Balanced adjustment agent etc..Conventional finish is made of 90% or more major constituent and 10% accessory constituent below, is used to adjusting jointly
Fine frictional behaviour prevents or eliminates accumulation of static electricity, assigns the performances such as smooth fiber, boundling, antistatic, soft.
Between the adjustable fiber of silk oiling agent and fiber, coefficient of friction between fiber and metal, reduce the electrostatic generated by friction,
Make fiber that there is good convergence, flatness and fiber separation, meets the needs of fiber post-processing concerned process steps.Ordinary circumstance
Under, polyamide spinning finisher is mainly made of wetting agent, collecting agent, smooth agent, emulsifier, antistatic agent etc..General filament yarn oil agent
Main function be that the fiber after oiling is enable successfully to be wound, silk cylinder forming, and in stretching process reduce lousiness,
Broken end guarantees normal stretch.It it requires that finish must have the wetability and fiber obvolvent of good antistatic property and appropriateness
Property, flatness, heat-resisting quantity, low volatility.Recently as the high speed of nylon industry spinning, fine-denier, the function of fiber
Change the development with greenization, higher performance requirement is proposed to the performance of polyamide spinning finisher.
But currently on the market there are following some deficiencies in existing polyamide spinning finisher mostly, comprising: the continuous synthetic fibre spinning having
Heat resistance, the inoxidizability of finish are poor, and inoxidizability is poor, tend to that nylon fibre is made to turn yellow, to cause great loss；
Emulsifier in some polyamide spinning finishers then contains APEO ingredient, and APEO is environmental hormone substance, this prints and dyes to downstream
The products export of enterprise causes difficulty, also will cause environmental pollution and ecological hazard；In addition, the extrusion spinning having currently on the market
The emulsibility of finish is poor, so that the finish on silk is not easy to be cleaned, to can impact to the dyeing in rear road.Especially
The antistatic property on ground, continuous synthetic fibre spinning oil needs to be further increased, and generallys use phosphate in the market as antistatic agent, this
It can guarantee that finish has good antistatic property under higher levels of humidity, but in the lower situation of humidity, antistatic effect is greatly
It reduces, this leads to often occur occurring winding, broken end because antistatic bad now in dry season or northern area
As.
Summary of the invention
The technical problems to be solved by the invention: for current spinning oil antistatic property difference and occur winding, broken end
Phenomenon, finish is easy to oxidize and the problem of causing fabric easily to turn yellow, a kind of anti-oxidant Antistatic spinning finish is provided.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of anti-oxidant Antistatic spinning finish, including following component, 100 ~ 150 parts of spinning oil-based materials, 1 ~ 3 part of lauric acid polyoxy second
Enester, 1 ~ 3 part of polyethylene glycol (PEG) oleate, 5 ~ 15 parts of antistatic activity agent, the smooth activating agent of 3 ~ 9 parts of spinning oils, 2 ~ 5 parts of oily antioxygens
Change activating agent；
The antistatic activity agent the preparation method comprises the following steps: taking phosphorus oxychloride 3 ~ 6:1 in mass ratio ~ 5:10 ~ 20 that propyl trichlorine is added
Silane, alcohol additive, are stirred in 40 ~ 50 DEG C, obtain mixture a, take mixture a 3 ~ 7:10 in mass ratio ~ 20 that diethyl is added
Glycol dimethyl ether is stirred in 100 ~ 110 DEG C, is cooled to room temperature, obtains cooled material, takes cooled material 2 ~ 5:10 ~ 15 in mass ratio
Dehydrated alcohol is added, stands, precipitating is taken to be evaporated under reduced pressure, it is dry to get antistatic activity agent.
The alcohol additive contracts the preparation method comprises the following steps: taking activated feedstock 2 ~ 6:5 in mass ratio ~ 8:50 ~ 70 that positive decyl is added
Water glycerin ether, deionized water, the catalyst for adding activated feedstock quality 5 ~ 10% are stirred, and are passed through hydrogen reaction, in
8MPa, 150 ~ 200 DEG C of 4 ~ 7h of holding, are cooled to room temperature, and filtering takes filtrate to get alcohol additive.
The activated feedstock are as follows: take D-sorbite, fructose, mannitol, galactooligosaccharide, maltose, it is any one in lactose
Kind or it is any it is several by any mass ratio mix to get.
The catalyst the preparation method comprises the following steps: according to the mass fraction, taking 10 ~ 15 parts of cerous nitrates, 3 ~ 7 parts of cobalt nitrates, 5 ~ 9 parts
Gallium nitrate, 80 ~ 100 parts of deionized waters, are stirred in 40 ~ 50 DEG C, obtain mixture, take mixture 20 ~ 50:3 ~ 5 in mass ratio
Tartaric acid is added, is warming up to 70 ~ 80 DEG C and is stirred, add the ethylene glycol of tartaric acid quality 20 ~ 30%, is stirred in 80 ~ 90 DEG C
Mixing filters, takes pumping filter residue and drying, calcines, is cooled to room temperature to get catalyst in 600 ~ 700 DEG C.
The smooth activating agent of spinning oil the preparation method comprises the following steps: take initial activity agent 5 ~ 9:1 in mass ratio ~ 4 be added pyridine,
Be passed through nitrogen dehydration keep 20 ~ 30min, obtain dehydrate, take propylene oxide 3 ~ 7:2 in mass ratio ~ 5 be added epoxy butane, then plus
The dehydrate for entering propylene oxide quality 2 ~ 9%, is passed through nitrogen protection, is warming up to 120 ~ 130 DEG C of heat preservations, is cooled to room temperature, obtains cooling
Object a takes cooled material a 40 ~ 50:2 in mass ratio ~ 5 that oxalic acid mixing is added, and through active carbon decoloring, filtering takes filtrate up to spinning oil
Smooth activating agent.
The initial activity agent are as follows: according to the mass fraction, take 5 ~ 10 parts of nutmeg amine, 3 ~ 7 parts of lauric acid, 1 ~ 4 part of octyl
Lauryl alcohol, 20 ~ 40 parts of propylene glycol, the mixing of 1 ~ 3 part of nonyl phenol to get.
The oil antioxidant activity agent the preparation method comprises the following steps: according to the mass fraction, taking 20 ~ 30 parts of core molecule activating agents, 5 ~ 8
Part triethylamine, 1 ~ 4 part of 4- lutidines, 40 ~ 60 parts of n,N-Dimethylformamide, are stirred in 20 ~ 25 DEG C, must stir mixed
Object is closed, takes stirring mixture 40 ~ 50:5 in mass ratio ~ 9 that antioxygen raw material is added, is stirred in 0 ~ 4 DEG C, is stirred then at 20 ~ 25 DEG C
Mixing is mixed, is evaporated under reduced pressure to get oily antioxidant activity agent.
The core molecule activating agent the preparation method comprises the following steps: take Putriscine 2 ~ 5:10 in mass ratio ~ 20 be added methanol, then
The methyl acrylate of methanol quality 20 ~ 30% is added, is stirred in 20 ~ 25 DEG C, is evaporated under reduced pressure, obtains vacuum distillation object, take decompression
Methanol is added in distillation 2 ~ 6:10 in mass ratio ~ 15, adds 2 ~ 4 times of methanol quality of Putriscine, stirs in 20 ~ 25 DEG C
Mixing is evaporated under reduced pressure to get core molecule activating agent.
The antioxygen raw material the preparation method comprises the following steps: take β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid in mass ratio 2 ~
5:10 ~ 20 be added n,N-Dimethylformamide, be stirred in 30 ~ 40 DEG C, add n,N-Dimethylformamide quality 10 ~
15% chlorobenzoyl chloride, is passed through nitrogen protection, is stirred in 30 ~ 40 DEG C, is evaporated under reduced pressure to get antioxygen raw material.
The spinning oil-based material are as follows: according to the mass fraction, take 5 ~ 10 parts of mineral oil, 1 ~ 3 part of amido silicon oil, 2 ~ 5 portions of castor-oil plants
Oil, the mixing of 5 ~ 10 parts of chemical fibre oil to get.
The present invention is compared with other methods, and advantageous effects are:
(1) antistatic activity agent prepared by the present invention is using alcohol additive as primary raw material, mainly through cerous nitrate, cobalt nitrate, nitre
Sour gallium etc., which carries out acid complexing gallium, can be used as the non-Dissociative CO molecule of active component, the work with CO insertion and C-C chain growth
With, enable in catalytic process that cobalt and gallium ion are evenly dispersed in atomic level in the lattice structure of perovskite, have compared with
Good catalytic activity carries out the catalytic hydrogenation to fructose, mannitol, galactooligosaccharide etc., improves alcohol conversion, draws as raw material
Entering polyol, and positive decyl glycidol ether is added under the conditions of base catalysis, alcohol activating agent dissociates alcohol anion,
Attack epoxide carries out open loop, generates ether compound, and silicon and the dual ignition-proof element of phosphorus are on the one hand introduced in spinning oil,
Fire-resisting protection is formed to fiber surface after oiling to spinning oil, on the other hand carries out phosphoric acid using phosphorus trichloride and ether compound
Change reaction, using obtaining that there is negative oxygen ion in product, there is preferable hygroscopicity and hydrophily, can preferably loss it is fine
The charge that dimension table face generates, so that antistatic effect improves；
(2) the smooth activating agent of spinning oil prepared by the present invention is with nutmeg amine, lauric acid etc. for initiator raw material, and epoxy is added
Propane, epoxy butane etc. are reacted, and the heat resistance that introducing propylene oxide chain link improves spinning oil is good, introduce short carbon chain
Initiator reduces spinning oil decomposition residual, so that the coking phenomenon in spinning surface is greatly lowered, to improve the hair of fiber
On the other hand silk, fracture of wire phenomenon introduce the biggish initiator raw material of viscosity, and subtract the intermolecular space steric hindrance of smooth activating agent
It is few, it intertwine with each other and increases between flexible macromolecular chain, by improving the viscosity of spinning oil, so that the oil film formed when its use is embraced
Resultant force and wear-resisting property are improved, and fiber are preferably adhered to, then arrange by the chain link of pfpe molecule chain, when reduction is sprawled
Surface tension form continuous oil film so that arrangement is close and carry out spinning protection；
(3) antioxygen raw material prepared by the present invention is with β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid for raw material, and benzene first is added
Acyl chlorides carries out acyl chloride reaction, adds the core molecule formed through Putriscine and methyl acrylate, and as grafting antioxygen
The end group amino of obtained acid chloride product and skeleton is carried out amidation condensation reaction, on the one hand existed by the skeleton structure of activating agent
Hindered phenol and two kinds of tertiary amine are introduced in spinning oil has the active group for removing free radical, plays length to the antioxygenic property of oil base
The protection of effect has preferable polarity and stability on the other hand using the amido bond introduced, by connecting antioxidant activity
Agent is kept antioxidative stabilizer during spinning oil is heated, and antioxidant is existed using the branched structure of skeleton structure
It is evenly dispersed in finish, improve spinning oil performance.
Specific embodiment
Catalyst the preparation method comprises the following steps: according to the mass fraction, taking 10 ~ 15 parts of cerous nitrates, 3 ~ 7 parts of cobalt nitrates, 5 ~ 9 parts of nitric acid
Gallium, 80 ~ 100 parts of deionized waters, are stirred 20 ~ 40min in 40 ~ 50 DEG C, obtain mixture, take mixture in mass ratio 20 ~ 50:
3 ~ 5 are added tartaric acid, are warming up to 70 ~ 80 DEG C and are stirred 30 ~ 60min, add the ethylene glycol of tartaric acid quality 20 ~ 30%, in
80 ~ 90 DEG C are stirred 3 ~ 6h, filter, take pumping filter residue and drying, in 600 ~ 700 DEG C of 3 ~ 5h of calcining, be cooled to room temperature to get catalysis
Agent.
Activated feedstock are as follows: take D-sorbite, fructose, mannitol, galactooligosaccharide, maltose, any one in lactose or
It is any it is several by any mass ratio mix to get.
Alcohol additive the preparation method comprises the following steps: take activated feedstock 2 ~ 6:5 in mass ratio ~ 8:50 ~ 70 be added positive decyl shrink it is sweet
Oily ether, deionized water, add the catalyst of activated feedstock quality 5 ~ 10%, are stirred 20 ~ 40min in 800r/min, are passed through
Hydrogen reaction, in 8MPa, 150 ~ 200 DEG C of 4 ~ 7h of holding, is cooled to room temperature, and filters, takes filtrate to get alcohol additive.
Antistatic activity agent the preparation method comprises the following steps: taking phosphorus oxychloride 3 ~ 6:1 in mass ratio ~ 5:10 ~ 20 that propyl trichlorine is added
Silane, alcohol additive are stirred 1 ~ 3h in 40 ~ 50 DEG C, obtain mixture a, and mixture a 3 ~ 7:10 in mass ratio ~ 20 is taken to be added
Diethylene glycol dimethyl ether is stirred 3 ~ 5h in 100 ~ 110 DEG C, is cooled to room temperature, obtains cooled material, take cooled material in mass ratio 2 ~
Dehydrated alcohol is added in 5:10 ~ 15, stands 30 ~ 50min, and precipitating is taken to be evaporated under reduced pressure, dry to get antistatic activity agent.
Initial activity agent are as follows: according to the mass fraction, take 5 ~ 10 parts of nutmeg amine, 3 ~ 7 parts of lauric acid, 1 ~ 4 part of octyl 12
Alcohol, 20 ~ 40 parts of propylene glycol, the mixing of 1 ~ 3 part of nonyl phenol to get.
The smooth activating agent of spinning oil the preparation method comprises the following steps: take initial activity agent 5 ~ 9:1 in mass ratio ~ 4 be added pyridine, be passed through
Nitrogen dehydration keeps 20 ~ 30min, obtains dehydrate, takes propylene oxide 3 ~ 7:2 in mass ratio ~ 5 that epoxy butane is added, adds ring
The dehydrate of Ethylene Oxide quality 2 ~ 9%, is passed through nitrogen protection, is warming up to 120 ~ 130 DEG C of 20 ~ 30min of heat preservation, is cooled to room temperature, obtains
Cooled material a takes cooled material a 40 ~ 50:2 in mass ratio ~ 5 that oxalic acid mixing is added, and through active carbon decoloring, filtering takes filtrate up to spinning
The smooth activating agent of silk oil.
Core molecule activating agent the preparation method comprises the following steps: take Putriscine 2 ~ 5:10 in mass ratio ~ 20 be added methanol, add
The methyl acrylate of methanol quality 20 ~ 30%, it is stirred 18 in 20 ~ 25 DEG C ~ for 24 hours, vacuum distillation obtains vacuum distillation object, takes and subtract
It presses distillation 2 ~ 6:10 in mass ratio ~ 15 that methanol is added, adds 2 ~ 4 times of methanol quality of Putriscine, stirred in 20 ~ 25 DEG C
Mixing 20 ~ for 24 hours is mixed, is evaporated under reduced pressure to get core molecule activating agent.
Antioxygen raw material the preparation method comprises the following steps: take β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid 2 ~ 5:10 in mass ratio ~
20 are added n,N-Dimethylformamide, are stirred 20 ~ 40min in 30 ~ 40 DEG C, add n,N-Dimethylformamide quality 10
~ 15% chlorobenzoyl chloride, is passed through nitrogen protection, and 3 ~ 7h is stirred in 30 ~ 40 DEG C, is evaporated under reduced pressure to get antioxygen raw material.
Oily antioxidant activity agent the preparation method comprises the following steps: according to the mass fraction, taking 20 ~ 30 portions of core molecule activating agents, 5 ~ 8 part three
Ethamine, 1 ~ 4 part of 4- lutidines, 40 ~ 60 parts of n,N-Dimethylformamide, are stirred 40 ~ 50min in 20 ~ 25 DEG C, must stir
Mixture is mixed, takes stirring mixture 40 ~ 50:5 in mass ratio ~ 9 that antioxygen raw material is added, is stirred 30 ~ 50min in 0 ~ 4 DEG C, then
It is stirred 10 ~ 12h in 20 ~ 25 DEG C, is evaporated under reduced pressure to get oily antioxidant activity agent.
Spinning oil-based material are as follows: according to the mass fraction, take 5 ~ 10 parts of mineral oil, 1 ~ 3 part of amido silicon oil, 2 ~ 5 parts of castor oil, 5 ~
The mixing of 10 parts of chemical fibre oil to get.
A kind of anti-oxidant Antistatic spinning finish, according to the mass fraction, including 100 ~ 150 parts of spinning oil-based materials, 1 ~ 3 portion of laurel
Sour polyoxyethylene ester, 1 ~ 3 part of polyethylene glycol (PEG) oleate, 5 ~ 15 parts of antistatic activity agent, the smooth activating agent of 3 ~ 9 parts of spinning oils, 2 ~ 5
The oily antioxidant activity agent of part.
Catalyst the preparation method comprises the following steps: according to the mass fraction, taking 10 parts of cerous nitrates, 3 parts of cobalt nitrates, 5 parts of gallium nitrates, 80 parts
Deionized water is stirred 20min in 40 DEG C, obtains mixture, takes mixture 20:3 in mass ratio that tartaric acid is added, is warming up to 70
DEG C it is stirred 30min, adds the ethylene glycol of tartaric acid quality 20%, be stirred 3h in 80 DEG C, filtered, takes that filter slag dry
It is dry, in 600 DEG C of calcining 3h, it is cooled to room temperature to get catalyst.
Activated feedstock are as follows: take D-sorbite, fructose by any mass ratio mix to get.
Alcohol additive the preparation method comprises the following steps: take activated feedstock 2:5:50 in mass ratio be added positive decyl glycidol ether, go
Ionized water, adds the catalyst of activated feedstock quality 5%, is stirred 20min in 800r/min, is passed through hydrogen reaction, in
8MPa, 150 DEG C of holding 4h, are cooled to room temperature, and filtering takes filtrate to get alcohol additive.
Antistatic activity agent the preparation method comprises the following steps: take phosphorus oxychloride 3:1:10 in mass ratio be added propyltrichlorosilan, alcohol
Additive is stirred 1h in 40 DEG C, obtains mixture a, takes mixture a 3:10 in mass ratio that diethylene glycol dimethyl ether is added, in
100 DEG C are stirred 3h, are cooled to room temperature, obtain cooled material, take cooled material 2:10 in mass ratio that dehydrated alcohol is added, and stand
30min takes precipitating to be evaporated under reduced pressure, dry to get antistatic activity agent.
Initial activity agent are as follows: according to the mass fraction, take 5 parts of nutmeg amine, 3 parts of lauric acid, 1 part of octyl dodecanol, 20 parts
Propylene glycol, the mixing of 1 part of nonyl phenol to get.
The smooth activating agent of spinning oil the preparation method comprises the following steps: take initial activity agent 5:1 in mass ratio be added pyridine, be passed through nitrogen
Dehydration keeps 20min, obtains dehydrate, takes propylene oxide 3:2 in mass ratio that epoxy butane is added, adds propylene oxide quality 2%
Dehydrate, be passed through nitrogen protection, be warming up to 120 DEG C of heat preservation 20min, be cooled to room temperature, obtain cooled material a, take cooled material a by matter
Oxalic acid mixing is added than 40:2 in amount, and through active carbon decoloring, filtering takes filtrate up to the smooth activating agent of spinning oil.
Core molecule activating agent the preparation method comprises the following steps: take Putriscine 2:10 in mass ratio be added methanol, add methanol
The methyl acrylate of quality 20% is stirred 18h in 20 DEG C, and vacuum distillation obtains vacuum distillation object, takes vacuum distillation object by matter
Methanol is added than 2:10 in amount, adds 2 times of methanol quality of Putriscine, is stirred 20h in 20 DEG C, is evaporated under reduced pressure, i.e.,
Obtain core molecule activating agent.
Antioxygen raw material the preparation method comprises the following steps: β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid 2:10 in mass ratio is taken to add
Enter n,N-Dimethylformamide, is stirred 20min in 30 DEG C, adds the benzoyl of n,N-Dimethylformamide quality 10%
Chlorine is passed through nitrogen protection, and 3h is stirred in 30 DEG C, is evaporated under reduced pressure to get antioxygen raw material.
Oily antioxidant activity agent the preparation method comprises the following steps: according to the mass fraction, take 20 portions of core molecule activating agents, 5 parts of triethylamines,
1 part of 4- lutidines, 40 parts of n,N-Dimethylformamide, are stirred 40min in 20 DEG C, obtain stirring mixture, take stirring
Antioxygen raw material is added in mixture 40:5 in mass ratio, is stirred 30min in 0 DEG C, and 10h is stirred then at 20 DEG C, and decompression is steamed
It evaporates to get oily antioxidant activity agent.
Spinning oil-based material are as follows: according to the mass fraction, take 5 parts of mineral oil, 1 part of amido silicon oil, 2 parts of castor oil, 5 parts of chemical fibre oil
Mixing to get.
A kind of anti-oxidant Antistatic spinning finish, according to the mass fraction, including 100 parts of spinning oil-based materials, 1 part of lauric acid polyoxy
Vinyl acetate, 1 part of polyethylene glycol (PEG) oleate, 5 parts of antistatic activity agent, the smooth activating agent of 3 parts of spinning oils, 2 parts of oily antioxidant activities
Agent.
Catalyst the preparation method comprises the following steps: according to the mass fraction, taking 12 parts of cerous nitrates, 5 parts of cobalt nitrates, 7 parts of gallium nitrates, 90 parts
Deionized water is stirred 30min in 45 DEG C, obtains mixture, takes mixture 35:4 in mass ratio that tartaric acid is added, is warming up to 75
DEG C it is stirred 45min, adds the ethylene glycol of tartaric acid quality 25%, be stirred 5h in 85 DEG C, filtered, takes that filter slag dry
It is dry, in 650 DEG C of calcining 4h, it is cooled to room temperature to get catalyst.
Activated feedstock are as follows: take mannitol, galactooligosaccharide by any mass ratio mix to get.
Alcohol additive the preparation method comprises the following steps: take activated feedstock 4:6:60 in mass ratio be added positive decyl glycidol ether, go
Ionized water, adds the catalyst of activated feedstock quality 8%, is stirred 30min in 800r/min, is passed through hydrogen reaction, in
8MPa, 175 DEG C of holding 5h, are cooled to room temperature, and filtering takes filtrate to get alcohol additive.
Antistatic activity agent the preparation method comprises the following steps: take phosphorus oxychloride 5:3:15 in mass ratio be added propyltrichlorosilan, alcohol
Additive is stirred 2h in 45 DEG C, obtains mixture a, takes mixture a 5:15 in mass ratio that diethylene glycol dimethyl ether is added, in
105 DEG C are stirred 4h, are cooled to room temperature, obtain cooled material, take cooled material 4:12 in mass ratio that dehydrated alcohol is added, and stand
40min takes precipitating to be evaporated under reduced pressure, dry to get antistatic activity agent.
Initial activity agent are as follows: according to the mass fraction, take 8 parts of nutmeg amine, 5 parts of lauric acid, 3 parts of octyl dodecanols, 30 parts
Propylene glycol, the mixing of 2 parts of nonyl phenols to get.
The smooth activating agent of spinning oil the preparation method comprises the following steps: take initial activity agent 7:3 in mass ratio be added pyridine, be passed through nitrogen
Dehydration keeps 25min, obtains dehydrate, takes propylene oxide 5:3 in mass ratio that epoxy butane is added, adds propylene oxide quality 5%
Dehydrate, be passed through nitrogen protection, be warming up to 125 DEG C of heat preservation 25min, be cooled to room temperature, obtain cooled material a, take cooled material a by matter
Oxalic acid mixing is added than 45:3 in amount, and through active carbon decoloring, filtering takes filtrate up to the smooth activating agent of spinning oil.
Core molecule activating agent the preparation method comprises the following steps: take Putriscine 4:15 in mass ratio be added methanol, add methanol
The methyl acrylate of quality 25% is stirred 21h in 22 DEG C, and vacuum distillation obtains vacuum distillation object, takes vacuum distillation object by matter
Methanol is added than 4:12 in amount, adds 3 times of methanol quality of Putriscine, is stirred 22h in 22 DEG C, is evaporated under reduced pressure, i.e.,
Obtain core molecule activating agent.
Antioxygen raw material the preparation method comprises the following steps: β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid 4:15 in mass ratio is taken to add
Enter n,N-Dimethylformamide, is stirred 30min in 35 DEG C, adds the benzoyl of n,N-Dimethylformamide quality 12%
Chlorine is passed through nitrogen protection, and 5h is stirred in 35 DEG C, is evaporated under reduced pressure to get antioxygen raw material.
Oily antioxidant activity agent the preparation method comprises the following steps: according to the mass fraction, take 25 portions of core molecule activating agents, 6 parts of triethylamines,
3 parts of 4- lutidines, 50 parts of n,N-Dimethylformamide, are stirred 45min in 23 DEG C, obtain stirring mixture, take stirring
Antioxygen raw material is added in mixture 45:7 in mass ratio, is stirred 40min in 2 DEG C, and 11h is stirred then at 23 DEG C, and decompression is steamed
It evaporates to get oily antioxidant activity agent.
Spinning oil-based material are as follows: according to the mass fraction, take 7 parts of mineral oil, 2 parts of amido silicon oils, 4 parts of castor oil, 8 parts of chemical fibre oil
Mixing to get.
A kind of anti-oxidant Antistatic spinning finish, according to the mass fraction, including 125 parts of spinning oil-based materials, 2 parts of lauric acid polyoxies
Vinyl acetate, 2 parts of polyethylene glycol (PEG) oleates, 10 parts of antistatic activity agent, the smooth activating agent of 6 parts of spinning oils, 4 parts of oily antioxidant activities
Agent.
Catalyst the preparation method comprises the following steps: according to the mass fraction, taking 15 parts of cerous nitrates, 7 parts of cobalt nitrates, 9 parts of gallium nitrates, 100
Part deionized water, is stirred 40min in 50 DEG C, obtains mixture, takes mixture 50:5 in mass ratio that tartaric acid is added, is warming up to
80 DEG C are stirred 60min, add the ethylene glycol of tartaric acid quality 30%, are stirred 6h in 90 DEG C, filter, take suction filtration slag
It is dry, in 700 DEG C of calcining 5h, it is cooled to room temperature to get catalyst.
Activated feedstock are as follows: take maltose, lactose by any mass ratio mix to get.
Alcohol additive the preparation method comprises the following steps: take activated feedstock 6:8:70 in mass ratio be added positive decyl glycidol ether, go
Ionized water, adds the catalyst of activated feedstock quality 10%, is stirred 40min in 800r/min, is passed through hydrogen reaction, in
8MPa, 200 DEG C of holding 7h, are cooled to room temperature, and filtering takes filtrate to get alcohol additive.
Antistatic activity agent the preparation method comprises the following steps: take phosphorus oxychloride 6:5:20 in mass ratio be added propyltrichlorosilan, alcohol
Additive is stirred 3h in 50 DEG C, obtains mixture a, takes mixture a 7:20 in mass ratio that diethylene glycol dimethyl ether is added, in
110 DEG C are stirred 5h, are cooled to room temperature, obtain cooled material, take cooled material 5:15 in mass ratio that dehydrated alcohol is added, and stand
50min takes precipitating to be evaporated under reduced pressure, dry to get antistatic activity agent.
Initial activity agent are as follows: according to the mass fraction, take 10 parts of nutmeg amine, 7 parts of lauric acid, 4 parts of octyl dodecanols, 40 parts
Propylene glycol, the mixing of 3 parts of nonyl phenols to get.
The smooth activating agent of spinning oil the preparation method comprises the following steps: take initial activity agent 9:4 in mass ratio be added pyridine, be passed through nitrogen
Dehydration keeps 30min, obtains dehydrate, takes propylene oxide 7:5 in mass ratio that epoxy butane is added, adds propylene oxide quality 9%
Dehydrate, be passed through nitrogen protection, be warming up to 130 DEG C of heat preservation 30min, be cooled to room temperature, obtain cooled material a, take cooled material a by matter
Oxalic acid mixing is added than 50:5 in amount, and through active carbon decoloring, filtering takes filtrate up to the smooth activating agent of spinning oil.
Core molecule activating agent the preparation method comprises the following steps: take Putriscine 5:20 in mass ratio be added methanol, add methanol
The methyl acrylate of quality 30% is stirred for 24 hours in 25 DEG C, and vacuum distillation obtains vacuum distillation object, takes vacuum distillation object by matter
Methanol is added than 6:15 in amount, adds 4 times of methanol quality of Putriscine, is stirred in 25 DEG C for 24 hours, vacuum distillation, i.e.,
Obtain core molecule activating agent.
Antioxygen raw material the preparation method comprises the following steps: β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid 5:20 in mass ratio is taken to add
Enter n,N-Dimethylformamide, is stirred 40min in 40 DEG C, adds the benzoyl of n,N-Dimethylformamide quality 15%
Chlorine is passed through nitrogen protection, and 7h is stirred in 40 DEG C, is evaporated under reduced pressure to get antioxygen raw material.
Oily antioxidant activity agent the preparation method comprises the following steps: according to the mass fraction, take 30 portions of core molecule activating agents, 8 parts of triethylamines,
4 parts of 4- lutidines, 60 parts of n,N-Dimethylformamide, are stirred 50min in 25 DEG C, obtain stirring mixture, take stirring
Antioxygen raw material is added in mixture 50:9 in mass ratio, is stirred 50min in 4 DEG C, and 12h is stirred then at 25 DEG C, and decompression is steamed
It evaporates to get oily antioxidant activity agent.
Spinning oil-based material are as follows: according to the mass fraction, take 10 parts of mineral oil, 3 parts of amido silicon oils, 5 parts of castor oil, 10 parts of chemical fibres
Oil mixing to get.
A kind of anti-oxidant Antistatic spinning finish, according to the mass fraction, including 150 parts of spinning oil-based materials, 3 parts of lauric acid polyoxies
Vinyl acetate, 3 parts of polyethylene glycol (PEG) oleates, 15 parts of antistatic activity agent, the smooth activating agent of 9 parts of spinning oils, 5 parts of oily antioxidant activities
Agent.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking antistatic activity agent.
Comparative example 2: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking the smooth activating agent of spinning oil.
Comparative example 3: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking oily antioxidant activity agent.
Comparative example 4: the anti-oxidant Antistatic spinning finish of Nanjing company production.
Embodiment is tested with anti-oxidant Antistatic spinning finish obtained by comparative example according to GB/T14342-1993, is tested
The results are shown in Table 1:
Table 1:
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Surface electrostatic (kv) | 0.07 | 0.08 | 0.12 | 0.10 | 0.18 | 0.20 | 0.28 |
| Oil applying rate (%) | 1.20 | 1.15 | 1.19 | 1.02 | 1.07 | 1.12 | 0.89 |
| Ultimate strength (g) | 53.1 | 52.5 | 51.6 | 52.9 | 51.9 | 52.3 | 48.6 |
| Inoxidizability | Preferably | Preferably | Preferably | Preferably | Generally | Generally | It is poor |
In summary, the resulting anti-oxidant Antistatic spinning finish of the present invention has good antistatic property, oils more uniform, compares
In commercial product, effect is more preferable, is worth promoting.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of anti-oxidant Antistatic spinning finish includes following component, 100 ~ 150 parts of spinning oil-based materials, 1 ~ 3 according to the mass fraction
Part lauric acid polyoxyethylene ester, 1 ~ 3 part of polyethylene glycol (PEG) oleate, which is characterized in that further include 5 ~ 15 parts of antistatic activity agent, 3 ~
The smooth activating agent of 9 parts of spinning oils, 2 ~ 5 parts of oily antioxidant activity agent；
The antistatic activity agent the preparation method comprises the following steps: taking phosphorus oxychloride 3 ~ 6:1 in mass ratio ~ 5:10 ~ 20 that propyl trichlorine is added
Silane, alcohol additive, are stirred in 40 ~ 50 DEG C, obtain mixture a, take mixture a 3 ~ 7:10 in mass ratio ~ 20 that diethyl is added
Glycol dimethyl ether is stirred in 100 ~ 110 DEG C, is cooled to room temperature, obtains cooled material, takes cooled material 2 ~ 5:10 ~ 15 in mass ratio
Dehydrated alcohol is added, stands, precipitating is taken to be evaporated under reduced pressure, it is dry to get antistatic activity agent.
2. anti-oxidant Antistatic spinning finish according to claim 1, which is characterized in that the preparation method of the alcohol additive
Are as follows: it takes activated feedstock 2 ~ 6:5 in mass ratio ~ 8:50 ~ 70 that positive decyl glycidol ether, deionized water is added, adds active original
The catalyst of material quality 5 ~ 10% is stirred, and is passed through hydrogen reaction, in 8MPa, 150 ~ 200 DEG C of 4 ~ 7h of holding, is cooled to room temperature,
Filtering, takes filtrate to get alcohol additive.
3. anti-oxidant Antistatic spinning finish according to claim 2, which is characterized in that the activated feedstock are as follows: take sorb
Sugar alcohol, fructose, mannitol, galactooligosaccharide, maltose, any one in lactose or it is any it is several mixed by any mass ratio,
To obtain the final product.
4. anti-oxidant Antistatic spinning finish according to claim 2, which is characterized in that the preparation method of the catalyst
Are as follows: according to the mass fraction, 10 ~ 15 parts of cerous nitrates, 3 ~ 7 parts of cobalt nitrates, 5 ~ 9 parts of gallium nitrates, 80 ~ 100 parts of deionized waters are taken, in 40
~ 50 DEG C are stirred, and obtain mixture, take mixture 20 ~ 50:3 in mass ratio ~ 5 that tartaric acid is added, are warming up to 70 ~ 80 DEG C of stirrings
Mixing, adds the ethylene glycol of tartaric acid quality 20 ~ 30%, is stirred in 80 ~ 90 DEG C, filters, pumping filter residue and drying is taken, in 600
~ 700 DEG C of calcinings, are cooled to room temperature to get catalyst.
5. anti-oxidant Antistatic spinning finish according to claim 1, which is characterized in that the smooth activating agent of spinning oil
The preparation method comprises the following steps: taking initial activity agent 5 ~ 9:1 in mass ratio ~ 4 that pyridine is added, it is passed through nitrogen dehydration and keeps 20 ~ 30min, obtain de-
Water object takes propylene oxide 3 ~ 7:2 in mass ratio ~ 5 that epoxy butane is added, adds the dehydrate of propylene oxide quality 2 ~ 9%, leads to
Enter nitrogen protection, be warming up to 120 ~ 130 DEG C of heat preservations, be cooled to room temperature, obtain cooled material a, take cooled material a 40 ~ 50:2 in mass ratio ~
5 are added oxalic acid mixing, and through active carbon decoloring, filtering takes filtrate up to the smooth activating agent of spinning oil.
6. anti-oxidant Antistatic spinning finish according to claim 5, which is characterized in that the initial activity agent are as follows: press matter
Number meter is measured, 5 ~ 10 parts of nutmeg amine, 3 ~ 7 parts of lauric acid, 1 ~ 4 part of octyl dodecanol, 20 ~ 40 parts of propylene glycol, 1 ~ 3 part of nonyl are taken
Phenol mixing to get.
7. anti-oxidant Antistatic spinning finish according to claim 1, which is characterized in that the system of the oil antioxidant activity agent
Preparation Method are as follows: according to the mass fraction, take 20 ~ 30 portions of core molecule activating agents, 5 ~ 8 parts of triethylamines, 1 ~ 4 part of 4- lutidines, 40 ~
60 parts of n,N-Dimethylformamide, are stirred in 20 ~ 25 DEG C, obtain stirring mixture, take stirring mixture in mass ratio 40 ~
Antioxygen raw material is added in 50:5 ~ 9, is stirred in 0 ~ 4 DEG C, is stirred then at 20 ~ 25 DEG C, and vacuum distillation is anti-oxidant to get oil
Activating agent.
8. anti-oxidant Antistatic spinning finish according to claim 7, which is characterized in that the preparation of the core molecule activating agent
Method are as follows: take Putriscine 2 ~ 5:10 in mass ratio ~ 20 that methanol is added, add the acrylic acid first of methanol quality 20 ~ 30%
Ester is stirred in 20 ~ 25 DEG C, and vacuum distillation obtains vacuum distillation object, and vacuum distillation object 2 ~ 6:10 in mass ratio ~ 15 is taken to be added
Methanol adds 2 ~ 4 times of methanol quality of Putriscine, is stirred in 20 ~ 25 DEG C, and vacuum distillation is living to get core molecule
Property agent.
9. anti-oxidant Antistatic spinning finish according to claim 7, which is characterized in that the preparation method of the antioxygen raw material
Are as follows: take β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid 2 ~ 5:10 in mass ratio ~ 20 that n,N-Dimethylformamide is added, in
30 ~ 40 DEG C are stirred, and add the chlorobenzoyl chloride of n,N-Dimethylformamide quality 10 ~ 15%, are passed through nitrogen protection, in 30 ~
40 DEG C are stirred, and are evaporated under reduced pressure to get antioxygen raw material.
10. anti-oxidant Antistatic spinning finish according to claim 1, which is characterized in that the spinning oil-based material are as follows: press matter
Measure number meter, take 5 ~ 10 parts of mineral oil, 1 ~ 3 part of amido silicon oil, 2 ~ 5 parts of castor oil, the mixing of 5 ~ 10 parts of chemical fibre oil to get.
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