CN101519847A - Short-fiber oil agent for aromatic polyamide fiber - Google Patents

Short-fiber oil agent for aromatic polyamide fiber Download PDF

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Publication number
CN101519847A
CN101519847A CN200910064514A CN200910064514A CN101519847A CN 101519847 A CN101519847 A CN 101519847A CN 200910064514 A CN200910064514 A CN 200910064514A CN 200910064514 A CN200910064514 A CN 200910064514A CN 101519847 A CN101519847 A CN 101519847A
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alkyl
weight
finish
acid ester
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CN101519847B (en
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张瑞波
李克文
时东兴
陈小民
杨玉敏
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China Petrochemical Corp
Sinopec Luoyang Guangzhou Engineering Co Ltd
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Sinopec Luoyang Petrochemical Engineering Corp
China Petrochemical Corp
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Abstract

The invention discloses a short-fiber oil agent for aromatic polyamide fiber, which is prepared from 3 to 40 weight percent of polyol fatty acid ester, 5 to 70 weight percent of polyoxyethylene polyol fatty acid ester, 5 to 40 weight percent of fatty alcohol ethylene oxide-propylene oxide random copolyether or polyether ester, 1 to 40 weight percent of fatty alcohol polyethenoxy ether organic phosphate salt, 1 to 30 weight percent of fatty alcohol polyethenoxy ether sulfuric acid ester salt and 0.1 to 10 weight percent of polyether modified silicon oil. The oil agent can solve the defects of the poor main performance, i.e. poor electrostatic resistance, poor heat resistance, poor saturation, and the like of the prior oil agent, aims to provide an aramid short-fiber oil agent which has excellent electrostatic resistance, smoothness, softness and dyeing uniformity, enables the aramid short fiber to have excellent post processing performance, and the like.

Description

A kind of short-fiber oil agent for aromatic polyamide fiber
Technical field
The present invention relates to contain the oxygen macromolecule mixture is the lubricant oil composite of feature as additive, particularly a kind of aromatic polyamide fibre short-fiber oil agent that is used for.
Background technology
Aromatic polyamide fibre (Aromatic polyamide fibers) is an aramid fiber, its molecule is direct and two line polymers that aromatic ring is formed by connecting by amido link, mainly contain two kinds, a kind of is aramid fiber 1313 (trade name of E.I.Du Pont Company is Nomex), chemical name is poly (Poly-m-phenylene isophthalamide, PMIA) fiber, molecular formula is:
It has good heat-resisting, firing resistance, can use more than 10 years down at 220 ℃, 260 ℃ of fabrics are indeformable, just progressively charing and not fusion more than 370 ℃, can make suit, racing car clothes, fire-entry suit, heat-resistant anticorrosive filter cloth or lining cloth etc., Flame Retardant Fibers or fire resistance fibre are otherwise known as; Another kind is Fanglun l414 (trade name of E.I.Du Pont Company is Kevlar, and Kev draws), chemical name be (the molecular formula PPTA is for Poly-p-phenylenetereDhthalamide, PPTA) fiber:
It has superhigh intensity, high-modulus and high temperature resistant, acid and alkali-resistance, premium properties such as in light weight, its intensity is 5~6 times of steel wire, modulus is 2~3 times of steel wire, and toughness is 2 times of steel wire, and weight only is about 1/5 of steel wire, under 560 ℃, do not decompose, do not melt, have good insulation performance and ageing resistace, very extensive in aspect purposes such as the fortifying fibre of high-performance cord fabric thread, protective materials, composite, high-strength ropes, metal fibre is otherwise known as.The discovery of aramid fiber, be considered to very important historical progress of material circle, two kinds of aramid fibers by du pont company respectively at generation nineteen sixty, the 1970's succeeded in developing, because of being mainly used in national defense industry and new high-tech industry, its production technology is holded in close confidence, existing production capacity mainly concentrates on the U.S., Japanese and European, worldwide production is about 100,000 tons at present, price reaches 30 dollars/Kg, and world demand amount in 2008 will reach more than 500,000 tons, the whole world presents the situation that increases rapidly to the demand of aramid fiber, and aramid fiber has entered the period of develop rapidly as a kind of emerging high-performance fiber.
Although the research and development of the aramid fiber of China are started late, but the exploitation of aramid fiber be listed in country " ten. five ", " 11. five " during the Industrialization Projects of chemical fibre industry emphasis tackling key problem and encourage growth, develop very rapid, domestic existing several companies are independently developed at present has the aramid fiber commercial plant of perfect knowledge property right in steady production, Yizheng Chemical Fiber Co., Ltd., SINOPEC is wherein arranged, Yantai, Shandong spandex factory, enterprises such as Guangdong Charming Co., Ltd., output was by 10 tons of/year 11000 tons/year of developing rapidly up till now in 2000, the production technology of aramid fiber 1313 is grasped substantially, and other many companies also build in plan.The production technology of Fanglun l414 is tackled key problems, the p-aramid fiber condensate of having finished at present 100 tons/year prepares the pilot scale research project, because the special performance of aramid fiber, make its finish used in spinning process be different from other chemical fibre spinning oil, it is researched and produced and still belongs to blank at home, aramid fiber manufacturing enterprise shows with finish mainly by du pont company, Japan bamboo our company, Supreme Being people company etc. provides, not only cost an arm and a leg, and result of use is the antistatic property in spinning and the subsequent process especially, holding can be not satisfactory with level and smooth performance, in the spinning process of back processing, be prone to collaring, the finish monomeric species is more single, and it is not biodegradable, be difficult to satisfy domestic existing manufacturing technique and product quality, producer needs a kind of spinning oil of excellent combination property, to adapt to the aramid fiber production technology of domestic-developed, improve its product quality, satisfy the demand of the different purposes of aramid fiber.
Because the special performance and the purposes of aramid fiber make its production technology and technology be in monopoly position and confidential state, comprise used finish always.The disclosed aramid fiber finish of USP5139873 is made up of smooth agent, emulsifying agent, antistatic additive etc., main component is: low viscosity ester series lubricant agent, unrighted acid polyoxyethylene ester and unsaturated fatty alcohol polyoxyethylene ether, alkylsulfonate or alkylphosphonic etc., the characteristics of this finish are the easy emulsification of emulsion, coefficient of friction between fiber and fiber, fiber and the metal is low, and the aramid fiber that spins has lasting antistatic behaviour.But the color jaundice had peculiar smell when the poor heat resistance of institute's invention finish, aramid fiber were used as if high temperature.Deficiency at the disclosed finish of USP5139873, finish of the present invention has mainly used polyol fatty acid ester, atactic polyether of fine heat-resisting performance etc., to improve the heat resistance of finish, characteristics are effectively to reduce the tar voltinism of finish, high temperature xanthochromia and finish free from extraneous odour at high temperature.
JP11172577 discloses a kind of aramid fiber finish, this finish is made up of organic phosphate, amido silicon oil and non-ionic surface active agent etc., is characterized in that the antistatic property of finish is good, and the institute aramid fiber silk surface of spinning is smooth, be easy to combing in the after-processing technology, but its flatness and holding can be relatively poor.Weak point at JP11172577, finish of the present invention adopts multiple smooth agent monomers such as polyol fatty acid ester, polyoxyethylene polyols fatty acid ester, atactic polyether and polyether modified silicon oil, effectively improve the flatness and the holding of finish, improve the back processability of finish.
The disclosed aramid fiber finish of USP4670343 mainly is made up of polyoxyethylene glycerine dibasic acid ester, this finish can effectively improve the frictional behavior of fiber surface, especially reduce the confficient of static friction between the fiber under the high contact pressure, have more performance when aramid fiber is used as tyre cord, promptly cord fabric has good sticking and property and DIMENSIONAL STABILITY.But use this finish to spin coefficient of kinetic friction height between aramid fiber silk and the metal, and the antistatic property of finish does not demonstrate fully.In the oil formula of the present invention except that the good compound smooth agent of serviceability, for strengthening the antistatic property of finish, two or more dissimilar antistatic additive have been used, ratio by adjusting different antistatic additive and the carbon number distribution in the antistatic additive molecule, the antistatic property of finish is found full expression, moreover, can effectively reduce the coefficient of kinetic friction between fiber and the metal by smooth agents such as use polyol fatty acid esters.
The present invention is according to aramid fiber molecular structure, production characteristics, purposes and the deficiency of now using finish, the finish of function admirables such as a kind of heat resistance, flatness, antistatic behaviour and dyeability, back processability is provided, the finish water solubility of monomer is strong, easy cleaning, biodegradable, can not cause any harm to environment and human body.
Summary of the invention
The present invention be directed to the shortcomings such as antistatic behaviour, holding and poor heat resistance of finish in the prior art, a kind of new short-fiber oil agent for aromatic polyamide fiber is proposed, this finish has good antistatic behaviour, holding, dyeing uniformity and back processability, and the aramid fiber short fiber that spins can suit as the demand of different purposes.
Short-fiber oil agent for aromatic polyamide fiber provided by the invention is composed of the following components:
(a) polyol fatty acid ester of 3~40 weight %;
(b) the polyoxyethylene polyols fatty acid ester of 5~70 weight %;
(c) fatty alcohol oxirane expoxy propane random copolymerization ether or the polyether ester of 5~40 weight %;
(d) the aliphatic alcohol polyoxyvinethene phosphate salt of 1~40 weight %;
(e) the polyoxyethylene alkyl ether sulfate salt of 1~30 weight %;
(f) polyether modified silicon oil of 0.1~10 weight %.
Wherein: component (a) is by polyalcohol and the synthetic ester of aliphatic acid, described polyalcohol is for being selected from a kind of in glycerol, trimethylolpropane, the pentaerythrite at least, when selecting two or more polyalcohol for use, in all polyalcohol gross weight glycerol content requirement less than 20%, all the other can be chosen wantonly, and aliphatic acid is C 4~C 24Aliphatic acid, described synthetic ester is the full ester of aliphatic acid, promptly the hydroxyl in the polyalcohol is esterified fully, its shared weight percentage in finish is 3~40 weight %, is preferably 10~30 weight %.
Component (b) is the addition product of monohydroxy partial fatty-acid ester of polyol or polyhydroxy partial fatty-acid ester of polyol and oxirane, polyalcohol comprises polyalcohols such as glycerol, sorbierite, pentaerythrite, the molal quantity of oxirane is 4~30, be preferably 10~20, its shared weight percentage in finish is 5~70 weight %, is preferably 20~50 weight %.
Component (c) is the copolyether or the polyether ester of oxirane and expoxy propane, and structural formula is suc as formula shown in (1), the formula (2):
Figure A200910064514D00061
Figure A200910064514D00071
R wherein 1Be C 4~C 18Alkyl, be preferably C 4~C 12Alkyl or be methylene (CH 2) q, q is 2 or 3; R 2Be H atom or C 4~C 24Alkyl, be preferably C 4~C 18Alkyl; R 3Be C 4~C 24Alkyl, be preferably C 6~C 12Alkyl; M is 5~200 number, is preferably 10~50; N is 10~160 number, is preferably 15~60; Z is 1 or 2.Its shared weight percentage in finish is 5~40 weight %, is preferably 15~30 weight %.
Component (d) is the alkyl polyoxyethylene ether phosphate ester salt, and its molecular formula is R 4(CH 2CH 2O) xOPO 3M or (R 4(CH 2CH 2O) xO) 2PO 2M, R in the formula 4Be C 2~C 36Alkyl, be preferably C 4~C 12Alkyl; X is 2~12, is preferably 3~9; M is alkali metallic sodium or potassium; Its shared weight percentage in finish is 1~40 weight %, is preferably 5~30 weight %.
Component (e) is a polyoxyethylene alkyl ether sulfate salt, and its molecular formula is R 5(CH 2CH 2O) yOSO 3M, R in the formula 5Be C 2~C 36Alkyl, be preferably C 4~C 18Alkyl; Y=2~16 are preferably 3~12; M is alkali metallic sodium or potassium; Its shared weight percentage in finish is 1~30 weight %, is preferably 5~20 weight %.
Component (f) is a polyether modified silicon oil, and its molecular formula is:
Figure A200910064514D00072
Me is a methyl in the formula, R 6Be C 1~C 10, be preferably C 2~C 6Methylene, structural formula is (CH 2) r, r is 1~10 integer in the formula, is preferably 2~6 integer, m2 and n2 are respectively 2~50 number, are preferably 4~30 number, and p and q are respectively 10~200 number, be preferably 20~120 number, its shared weight percentage in finish is 0.1~10 weight %, is preferably 0.5~8 weight %.
Aromatic polyamide fibre short fiber of the present invention with the preparation method of finish is: add (a) and (b), (c) each component in reactor successively, 30~40 ℃ were stirred 20 minutes down, add (d), (e), (f) then, stirred again 20 minutes under 30~40 ℃, promptly get finish of the present invention.
Compared with prior art, short-fiber oil agent for aromatic polyamide fiber provided by the present invention, polyol fatty acid ester, atactic polyether or the polyether ester etc. of fine heat-resisting performance have mainly been used, to improve the heat resistance of finish, characteristics are effectively to reduce the tar voltinism of finish, high temperature xanthochromia, and finish free from extraneous odour at high temperature solve the relatively poor problem of heat resistance of now using finish; The multiple smooth agent monomer such as polyol fatty acid ester, polyoxyethylene polyols fatty acid ester, atactic polyether or polyether ester and polyether modified silicon oil etc. that adopts effectively improves the flatness and the holding of finish, improves the back processability of finish.In the oil formula of the present invention except that the good compound smooth agent of serviceability, for strengthening the antistatic property of finish, two or more dissimilar antistatic additive have been used, ratio by adjusting different antistatic additive and the carbon number distribution in the antistatic additive molecule, the antistatic property of finish is found full expression, moreover, can effectively reduce the coefficient of kinetic friction between fiber and the metal, thereby reduce the generation of static by smooth agents such as use polyol fatty acid esters.
The occupation mode of oil agent composition of the present invention is that oil tanker oils or utilizes nozzle directly to oil.
The specific embodiment
Describe the present invention in detail with specific embodiment below, but these embodiment do not limit the scope of the invention.
Embodiment 1
Get 20 gram pentaerythrite pelargonates, 20 gram polyoxyethylene (molal quantity is 10) glycerol dioleic acid esters, 30 gram polyethers (m=10, n=20, R 1Be n-octyl, R 2Be the H atom, z=1) in synthesis reactor, fully stirred 20 minutes down at 30 ± 2 ℃; Add 10 gram alkyl polyoxyethylene ether phosphate ester salt (R then successively 4Be C 8Alkyl, M are metallic element potassium, X=3), and 19 gram polyoxyethylene alkyl ether sulfate salt, (R 5Be C 6Alkyl, M are metallic element potassium, Y=6), and 1 gram polyether modified silicon oil (R 6Be C 4Hydrocarbon support, m2=10, n2=10, p=40, q=60 r=4), fully stirred 20 minutes down at 30 ± 2 ℃ then, filtered and promptly got the invention finish A of institute.
Embodiment 2
Get 30 gram PETO, 20 gram polyoxyethylene (molal quantity is 20) glycerol dioleic acid esters, 20 gram polyethers (m=20, n=40, R 1Be normal-butyl, R 2Be the H atom, z=1) in synthesis reactor, fully stirred 20 minutes down at 30 ± 2 ℃; Add 15 gram alkyl polyoxyethylene ether phosphate ester salt (R then successively 4Be C 12Alkyl, M are metallic element potassium, X=6), and 12 gram polyoxyethylene alkyl ether sulfate salt, (R 5Be C 12Alkyl, M are metallic element potassium, Y=6), and 3 gram polyether modified silicon oil (R 6Be C 4Hydrocarbon support, m2=20, n2=20, p=40, q=80 r=4), fully stirred 20 minutes down at 30 ± 2 ℃ then, filtered and promptly got the invention finish B of institute.
Embodiment 3
Get 30 gram pentaerythrite decylates, 20 gram polyoxyethylene (molal quantity is 20) sorbitan mono-laurates, 20 gram polyethers (m=20, n=40, R 1Be normal-butyl, R 2Be 12 alkyl, z=1) in synthesis reactor, fully stirred 20 minutes down at 30 ± 2 ℃; Add 15 gram alkyl polyoxyethylene ether phosphate ester salt (R then successively 4Be C 12Alkyl, M are metallic element potassium, X=6), and 12 gram polyoxyethylene alkyl ether sulfate salt, (R 5Be C 12Alkyl, M are metallic element potassium, Y=6), and 3 gram polyether modified silicon oil (R 6Be C 2Hydrocarbon support, m2=30, n2=20, p=40, q=40 r=2), fully stirred 20 minutes down at 30 ± 2 ℃ then, filtered and promptly got the invention finish C of institute.
Embodiment 4
Get 30 gram pentaerythrite palmitates, 20 gram polyoxyethylene (molal quantity is 20) glycerol dioleic acid esters, 20 gram polyethers (m=40, n=20, R 1Be normal-butyl, R 2Be the H atom, z=1) in synthesis reactor, fully stirred 20 minutes down at 30 ± 2 ℃; Add 15 gram alkyl polyoxyethylene ether phosphate ester salt (R then successively 4Be C 12Alkyl, M are metallic element potassium, X=6), and 12 gram polyoxyethylene alkyl ether sulfate salt, (R 5Be C 12Alkyl, M are metallic element potassium, Y=6), and 3 gram polyether modified silicon oil (R 6Be C 2Hydrocarbon support, m2=10, n2=10, p=40, q=120 r=2), fully stirred 20 minutes down at 30 ± 2 ℃ then, filtered and promptly got the invention finish D of institute.
Embodiment 5
Get 20 gram tricarboxymethyl propane oleates, 50 gram polyoxyethylene (molal quantity is 20) glycerol monoleates, 15 gram polyethers (m=50, n=60, R 1Be normal-butyl, R 2Be the H atom, z=1) in synthesis reactor, fully stirred 20 minutes down at 40 ± 2 ℃; Add 8 gram alkyl polyoxyethylene ether phosphate ester salt (R then successively 4Be C 12Alkyl, M are metallic element potassium, X=7), and 6 gram polyoxyethylene alkyl ether sulfate salt, (R 5Be C 12Alkyl, M are metallic element potassium, Y=9), and 1 gram polyether modified silicon oil (R 6Be C 6Hydrocarbon support, m2=10, n2=10, p=40, q=120 r=6), fully stirred 20 minutes down at 30 ± 2 ℃ then, filtered and promptly got the invention finish E of institute.
Embodiment 6
Get 10 gram trimethylolpropane laurates, 20 gram polyoxyethylene (molal quantity is 20) glycerol monoleates, 20 gram polyethers (m=30, n=10, R 1Be octadecyl, R 2Be dodecyl, z=1) in synthesis reactor, fully stirred 20 minutes down at 40 ± 2 ℃; Add 30 gram alkyl polyoxyethylene ether phosphate ester salt (R then successively 4Be C 12Alkyl, M are metallic element potassium, X=3), and 12 gram polyoxyethylene alkyl ether sulfate salt, (R 5Be C 12Alkyl, M are metallic element potassium, Y=6), and 8 gram polyether modified silicon oil (R 6Be C 2Hydrocarbon support, m2=20, n2=10, p=40, q=10 r=2), fully stirred 20 minutes down at 30 ± 2 ℃ then, filtered and promptly got the invention finish F of institute.
Embodiment 7
Get 10 gram trimethylolpropane caprylate, 10 gram pentaerythrite laurates, 15 gram polyoxyethylene (molal quantity is 15) glycerol monoleates, 15 gram polyethers (m=20, n=60, R 1Be octadecyl, R 2Be dodecyl, z=1) in synthesis reactor, fully stirred 20 minutes down at 35 ± 2 ℃; Add 30 gram alkyl polyoxyethylene ether phosphate ester salt (R then successively 4Be C 12Alkyl, M are metallic element potassium, X=3), and 12 gram polyoxyethylene alkyl ether sulfate salt, (R 5Be C 12Alkyl, M are metallic element potassium, Y=6), and 8 gram polyether modified silicon oil (R 6Be C 2Hydrocarbon support, m2=20, n2=10, p=40, q=10 r=2), fully stirred 20 minutes down at 40 ± 2 ℃ then, filtered and promptly got the invention finish G of institute.
Embodiment 8
Get 20 gram trimethylolpropane ricinoleate esters, 10 gram pentaerythrite n-caproates, 35 gram polyoxyethylene (molal quantity is 20) glycerol dioleic acid esters, 22 gram polyethers (m=30, n=38, R 1, R 2Be normal-butyl, z=1) in synthesis reactor, fully stirred 20 minutes down at 35 ± 2 ℃; Add 5 gram alkyl polyoxyethylene ether phosphate ester salt (R then successively 4Be C 8Alkyl, M are metallic element potassium, X=9), and 5 gram polyoxyethylene alkyl ether sulfate salt, (R 5Be C 18Alkyl, M are metallic element sodium, Y=16), and 3 gram polyether modified silicon oil (R 6Be C 3Hydrocarbon support, m2=5, n2=5, p=60, q=20 r=3), fully stirred 20 minutes down at 35 ± 2 ℃ then, filtered and promptly got the invention finish H of institute.
Embodiment 9
Get 5 gram trimethylolpropane stearates, 5 gram pentaerythritol stearates, 10 gram polyoxyethylene (molal quantity is 20) sorbitan monooleates, 15 gram polyethers (m=10, n=15, R 1, R 2Be 12 alkyl, z=1) in synthesis reactor, fully stirred 20 minutes down at 35 ± 2 ℃; Add 30 gram alkyl polyoxyethylene ether phosphate ester salt (R then successively 4Be C 8Alkyl, M are metallic element sodium, X=6), and 30 gram polyoxyethylene alkyl ether sulfate salt, (R 5Be C 12Alkyl, M are metallic element sodium, Y=6), and 5 gram polyether modified silicon oil (R 6Be C 3Hydrocarbon support, m2=5, n2=5, p=60, q=20 r=3), fully stirred 20 minutes down at 35 ± 2 ℃ then, filtered and promptly got the invention finish I of institute.
Embodiment 10
Get 30 gram trihydroxy methyl laurates, 30 gram polyoxyethylene (molal quantity is 20) sorbitan monostearates, 15 gram polyether ester (m=35, n=30, R 1Be n-octyl, R 3Be 20 alkyl, z=1) in synthesis reactor, fully stirred 20 minutes down at 35 ± 2 ℃; Add 7 gram alkyl polyoxyethylene ether phosphate ester salt (R then successively 4Be C 8Alkyl, M are metallic element sodium, X=7), and 10 gram polyoxyethylene alkyl ether sulfate salt, (R 5Be C 14Alkyl, M are metallic element sodium, Y=12), and 8 gram polyether modified silicon oil (R 6Be C 5Hydrocarbon support, m2=15, n2=15, p=40, q=20 r=3), fully stirred 20 minutes down at 35 ± 2 ℃ then, filtered and promptly got the invention finish J of institute.
Embodiment 11
Get 30 gram pentaerythrite laurates, 20 gram polyoxyethylene (molal quantity is 20) sorbitan mono-laurates, 30 gram polyether ester (m=30, n=30, R 1Be n-hexyl, R 3Be 18 alkyl, z=1) in synthesis reactor, fully stirred 20 minutes down at 35 ± 2 ℃; Add 10 gram alkyl polyoxyethylene ether phosphate ester salt (R then successively 4Be C 12Alkyl, M are metallic element sodium, X=6), and 9.5 gram polyoxyethylene alkyl ether sulfate salt, (R 5Be C 18Alkyl, M are metallic element sodium, Y=10), and 0.5 gram polyether modified silicon oil (R 6Be C 5Hydrocarbon support, m2=30, n2=30, p=60, q=30 r=6), fully stirred 20 minutes down at 35 ± 2 ℃ then, filtered and promptly got the invention finish K of institute.
Embodiment 12
Get 30 gram trihydroxy methyl laurates, 20 gram polyoxyethylene (molal quantity is 20) sorbitan monostearates, 20 gram polyethers (m=20, n=30, R 1, R 2Be n-octyl, z=2) in synthesis reactor, fully stirred 20 minutes down at 35 ± 2 ℃; Add 15 gram alkyl polyoxyethylene ether phosphate ester salt (R then successively 4Be C 12Alkyl, M are metal unit potassium, X=4), and 10 gram polyoxyethylene alkyl ether sulfate salt, (R 5Be C 8Alkyl, M are metallic element sodium, Y=10), and 5 gram polyether modified silicon oil (R 6Be C 5Hydrocarbon support, m2=15, n2=15, p=30, q=20 r=2), fully stirred 20 minutes down at 35 ± 2 ℃ then, filtered and promptly got the invention finish L of institute.
The assay method simple declaration
Measure heat resistance, film strength and the coefficient of friction etc. of embodiment 1~embodiment 12 prepared 12 finish samples in the laboratory, the result is as shown in table 1:
Table 1 oil performance
Figure A200910064514D00111
1. the test of smoldering: take by weighing sample 10.0 and restrain in the 50ml beaker, place electric jacket to heat in this beaker, observe temperature and the amount of being fuming size when smoldering continuously
2. hot plate test: measure sample 1.0ml and drip in No. 45 steel test pieces, this test piece is positioned in the baking oven, 220 ℃ of following constant temperature 3 minutes, be cooled to 30 ℃ then, observe the coking behavior of finish, " excellent " represents seldom coking, and " very " represents to have a small amount of coking
3. volatilization test: take by weighing sample 2.0 and restrain in the 50ml beaker, this beaker is positioned in the baking oven,, be cooled to 25 ℃ then, weigh and calculate the volatile quantity of finish 220 ± 2 ℃ of following constant temperature 2 hours.
The use of finish
Finish of the present invention is applied in the spinning production technology of the aromatic polyamide staple fibre that oils with the emulsion state.
1. finish occupation mode:
Oil tanker oils or nozzle oils.
2. finish operating position: choose several representational finishes and carry out commerical test, the results are shown in Table 2.
Table 2 finish result on trial
By table 1~table 2 data as can be known, from embodiment 1 to embodiment 12, the heat resistance of finish (amount of being fuming, tar voltinism, volatile quantity) is good, film strength and open flash point height, and coefficient of friction is low.
Free from extraneous odour in the finish use procedure oils evenly, and tow intensity and fiber be than resistance value height, rear processing Function admirable. Heat resistance, antistatic behaviour, holding and flatness that finish of the present invention has been described are good, table Now little for the amount of being fuming of finish, the tarring degree is low, oils evenly institute's spinning bundle powerful and compare resistance value Height, the rear processing characteristics of finish is good.

Claims (9)

1. a short-fiber oil agent for aromatic polyamide fiber is characterized in that this finish is composed of the following components, in the finish gross weight:
(a) polyol fatty acid ester of 3~40 weight %;
(b) the polyoxyethylene polyols fatty acid ester of 5~70 weight %;
(c) fatty alcohol oxirane expoxy propane random copolymerization ether or the polyether ester of 5~40 weight %;
(d) the aliphatic alcohol polyoxyvinethene phosphate salt of 1~40 weight %;
(e) the polyoxyethylene alkyl ether sulfate salt of 1~30 weight %;
(f) polyether modified silicon oil of 0.1~10 weight %;
Wherein: component (a) is by the synthetic ester of polyalcohol and aliphatic acid, and described polyalcohol is for being selected from glycerol, the trihydroxy methyl a kind of in alkane, the pentaerythrite at least, and aliphatic acid is C 4~C 24Aliphatic acid;
Component (b) is the addition product of monohydroxy partial fatty-acid ester of polyol or polyhydroxy partial fatty-acid ester of polyol and oxirane, and the molal quantity of oxirane is 4~30;
Component (c) is the copolyether or the polyether ester of oxirane and expoxy propane, and structural formula is suc as formula shown in (1), the formula (2):
Figure A200910064514C00021
Figure A200910064514C00022
R 1Be C 4~C 18Alkyl or be methylene (CH 2) q, q is 2 or 3, R 2, R 3Be C 4~C 24Alkyl, m is 5~200 number, n is 10~160 number, z is 1 or 2;
Component (d) is the alkyl polyoxyethylene ether phosphate ester salt, and its molecular formula is R 4(CH 2CH 2O) xOPO 3M or (R 4(CH 2CH 2O) xO) 2PO 2M, R in the formula 4Be C 2~C 36Alkyl, X=2~12, M is alkali metallic sodium or potassium;
Component (e) is a polyoxyethylene alkyl ether sulfate salt, and its molecular formula is R 5(CH 2CH 2O) yOSO 3M, R in the formula 5Be C 2~C 36Alkyl, Y=2~16, M is alkali metallic sodium or potassium;
Component (f) is a polyether modified silicon oil, and its molecular formula is:
Me is a methyl in the formula, and R is methyl or ethyl, R 6Be C 1~10Methylene, structural formula is (CH 2) r, r is 1~10 integer in the formula, and m2 and n2 are respectively 2~50 number, and p and q are respectively 10~200 number.
2. finish according to claim 1, it is characterized in that: the content of component (a) is 10~30 weight %, the content of component (b) is 20~50 weight %, the content of component (c) is 15~30 weight %, the content of component (d) is 5~30 weight %, the content of component (e) is 5~20 weight %, and the content of component (f) is 0.5~8 weight %, in the finish gross weight.
3. finish according to claim 1 and 2 is characterized in that: in the described polyol fatty acid ester molecule of component (a), contained all hydroxyls of its polyalcohol molecule are esterified fully.
4. finish according to claim 1 and 2 is characterized in that: in the described polyoxyethylene polyols fatty acid ester of component (b) molecule, and all hydroxylic moiety esterifications that its polyalcohol molecule is contained.
5. finish according to claim 1 and 2 is characterized in that: component (b) is the addition product of monohydroxy partial fatty-acid ester of polyol or polyhydroxy partial fatty-acid ester of polyol and oxirane, and the molal quantity of oxirane is 10~20.
6. finish according to claim 1 and 2 is characterized in that: the m in the component (c) is the number between 10~50, and n is 15~60 number, the R in the formula (2) 3Be C 6~C 12Alkyl.
7. finish according to claim 1 and 2 is characterized in that: the R in the component (d) 4Be C 4~C 12Alkyl, X is 3~9 number.
8. finish according to claim 1 and 2 is characterized in that: the R in the component (e) 5Be C 4~C 18Alkyl, Y is 3~12 number.
9. finish according to claim 1 and 2 is characterized in that: R in the component (f) 6Be C 2~6Methylene, r is 2~6 integer, m2 and n2 are respectively 4~30 number, p and q are respectively 20~120 number.
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