CN103437186A - Preparation method of high-speed polyester POY (Pre-Oriented Yarn) spinning oil agent - Google Patents
Preparation method of high-speed polyester POY (Pre-Oriented Yarn) spinning oil agent Download PDFInfo
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Abstract
The invention provides a preparation method of a high-speed polyester POY (Pre-Oriented Yarn) spinning oil agent. A pure oil agent except for water in the oil agent is composed of a main body part and an additive, wherein the main body part includes over 20 kinds of polyether compounds and the rest components belong to non-polyether additive. The preparation method comprises the following steps: firstly, metering the main body component of the oil agent, pumping the main body component into a reaction kettle in vacuum, stirring, heating to 50-70 DEG C, stirring, metering the additive components and water, and adding the metered additive components and water into the reaction kettle, stirring, heating to 70-80 DEG C, keeping the temperature for 40-50min, closely filter-pressing a product, and subpackaging the product after the product is checked to be qualified. The oil agent prepared by using the method provided by the invention is suitable for high-speed polyester POY spinning and a production process of a subsequent deform yarn; the oil agent endows the fiber good smoothness and bundling and favorable total viscosity-temperature and viscosity-concentration characteristics; the fiber is few in broken filament breaks, even and uniform in dyeing in the later drafting process; the smoke formation amount of a hot processing tank is small, generated white powder and coke amount are small and the cleaning period is long; a product is good in quality and stability.
Description
Technical field
The present invention relates to the finish used in a kind of synthetic fiber spinning process process, be specifically related to a kind of preparation method of polyester POY high-speed spin finishes.
Background technology
China is called terylene by the trade name of PET polyester (polyethylene terephthalate) silk goods.Terylene spinning generally adopts high speed spinning-draw-teisting technique at home, be pre-oriented yarn or partially oriented yarn (POY, Pre-Oriented Yarn or Partially Oriented Yarn) and draw textured yarn (DTY) (DTY, Draw Texturing Yarn) two step combinations, be called for short POY – DTY technique.For making polyester POY that the higher degree of orientation and degree of crystallinity be arranged, spinning speed usually will be in 3000 ~ 4600 m/min scopes, and spinning speed is fast, and production efficiency also improves thereupon.Flatness, convergence and antistatic property that the spinning oil that the requirement of polyester POY high speed spinning is used will have, to guarantee that tow is shaped, obvolvent appropriate, the lousiness little breakage.In addition, follow-up DTY operation will be carried out under 190 ~ 210 ℃ of high temperature, requires spinning oil should have enough good heat resistance, is difficult for again coking on hot plate.The polyether compound that oxirane and expoxy propane ring-opening polymerization obtain, due to its good seeping at high temperature greasy property and the thermal decomposition performance only selection of desirable finish main body component just.
Over nearly 40 years, the external polyester POY high-speed spin finishes used all turns to take polyethers as key component, as Japanese T – 2800, and the FT – 621 of the U.S. and German K – 105 etc.Jiangsu Tianyin chemical Co., Ltd is since 1980 mid-nineties 90s, adhere to carrying out the effort of polyester POY high-speed spin finishes production domesticization always, once in industry release and take YDG – 2000A polyester POY high-speed spin finishes (gold autumn, fine chemical material and the intermediate that polyethers is key component, 2004
12: 19 ~ 21,15).
The problem that polyester POY high-speed spin finishes ubiquity at present is: the sticky dense characteristic of the sticky temperature of many polyether monomers is desirable not enough, the monomer molecule amount is excessive, under low temperature, viscosity is large, causes to oil irregularly, and under high temperature, viscosity is little, finish on fiber can splash on hot-rolling under centrifugal action, be heated for a long time and easily cause the formation of burnt shape thing, light affect the heat conduction efficiency of heater, cause tow to stretch uneven, heavy lousiness and broken end are increased, impact is produced.And the monomer molecule amount is smaller, the viscosity jump phenomenon is generally arranged, cause the viscosity fluctuation scope in the high speed spinning process excessive, can cause equally to oil irregularly, on hot plate, coking amount is large, the quality of impact silk.
Terylene POY – DTY technique is from wire drawing oils the twisting winding process, along with constantly being heated and the moisture evaporation, the oil concentration on fiber top layer constantly increases from 10% left and right, until approach anhydrous state, therebetween some polyether compound in finish, particularly those are at the high monomer component of atactic polyether segment polyoxy isopropyl support content, be easy to occur being separated in certain concentration and temperature range, form the anti-thixotropic flow build emulsion of shear thickening.And fiber when high-speed cruising each other and rub with metal or with ceramic surface, the finish that is attached to fiber surface can be subject to strong shear action, these polyether component in its emulsion, will high viscosity and high coagulant state viscosity jump in other words occur in different separately temperature and concentration interval.This phenomenon not only exists in the experiment of some single polyether compound, has also obtained confirmation (Gao Laibao, Ge Jijun: Tianjin Textile Industry College journal, 1993,12 (3): 41 ~ 44) from the experiment of T – 2800 finishes to the loose our company of Japan.Avoid the generation of viscosity jump phenomenon, need to increase active component each other in the finish component and they and water between intermiscibility, prevent from occurring being separated in the fiber process process as far as possible, and the viscosity fluctuation of single polyether compound in component need to be reduced to minimum degree to the impact of finish integral body.
Summary of the invention
The object of the invention is to overcome and take the above weak point of the polyester POY high-speed spin finishes that polyethers is key component, provide a kind of preparation method of polyester POY high-speed spin finishes, further to improve the serviceability of this class finish in polyester POY high speed spinning process.The inventive method provide for the polyester POY high-speed spin finishes, meet such imagination and requirement fully, can avoid the generation of viscosity jump phenomenon, prevent from occurring being separated in the fiber process process, and in component, the viscosity fluctuation of single polyether compound is reduced to minimum degree to the impact of finish integral body.
The present invention is by the following technical solutions:
A kind of preparation method for the polyester POY high-speed spin finishes, it is characterized in that, by the main body component polyether compound of finish press rate of charge by each hold-up vessel through flowmeter accurate-metering vacuum suction reactor, stirring is warming up to 50 ~ 70 ℃, continue to stir 20 ~ 60 minutes, then add the additive component of finish by formula metering; After adding a certain amount of water, stirring is warming up to 70 ~ 80 ℃, maintains 40 ~ 50 minutes, and material in still is put into to airtight filter circulation press filtration to clear, and discharging is to the finished product basin, and product by analysis after the assay was approved, is sent the mixing kettle barrelling to;
Pure finish outside described finish dewaters is comprised of main part and additive; The main part of described finish is comprised of various ingredients more than 20 kinds polyether compound with various structures, accounts for 70 ~ 92% of pure finish gross mass; All the other components are additive, account for pure finish gross mass 8 ~ 30%.The molecular weight of pure finish all components is all below 4000, and wherein 80% between 600 ~ 2800.Because component is many, and have separately specific molecular structure, molecular weight ranges is wider, and between the finish system component, compatibility and resistance to overturning are good.
The described polyether compound that forms the finish main part has following general formula molecular structure:
RO[(EO)
x/(PO)
y]R’
Initial end group R and terminal groups R ' are H, or C
1~ C
18alkyl or aryl, or for thering is acyl group or the amide groups of corresponding carbon number, also or be inorganic acid radical.R and R ' can be identical or different, are in most of the cases not identical.[(EO)
x/ (PO)
y] be the polyether segment formed by oxygen ethylene group (EO) and oxygen isopropyl support group (PO), EO=-CH
2cH
2o-, PO=-CH
2cHMeO-or-CHMeCH
2o-.Polyether segment can be pure polyoxyethylene ether chain (EO)
xor polyoxy isopropyl support ether chain (PO)
y, can be also random (copolymerization) polyether chain formed by EO and PO, the random admixtured polyether chain of block polyether chain or block.X and y are respectively the molal quantity of EO and PO, and one of them may be zero.In the atactic polyether segment, x and y are respectively the total mole numbers of EO and PO.
Described class polyether compound molecular composition and structure separately, comprise that the sequential structure of strand is different, mainly as smooth agent, emulsifying agent, antistatic additive and other function ingredients.Initial end group, polyether segment and terminal groups in the polyether compound molecular structure is different to the effect of oil performance.When polyether compound is used as smooth agent, emulsifying agent, antistatic additive or other function ingredients, its initial end group, polyether segment and terminal groups must have the change adapted with appellative function aspect the Nomenclature Composition and Structure of Complexes (comprising micro-structural).
The main component of spinning oil is lubricant, in textile industry, is commonly called as smooth agent.Most basic function requirement for spinning oil is lubrication, even also the flatness of fiber is good.The high speed PET spinning speed requires finish to have fabulous permeability, and finish emulsion can be sprawled rapidly on the new surface of fiber.After oiling, the lubricated main fluid lubrication that leans on of fiber, therefore in general, the monomer component that viscosity is less more is conducive to improve the flatness of fiber.But monomer viscosity is too little, can cause the tow work in-process to be dispersed, convergence is bad, can affect equally carrying out smoothly of manufacturing procedure.Take into account flatness and the convergence of fiber, just must control viscosity and the mobility of finish well.In terylene POY – DTY technical process, the oil concentration that is applied to the fiber top layer can constantly be concentrated with the moisture evaporation owing to being heated, but when temperature raises, if most of component of finish can keep its sticky gentle sticky dense characteristic not occur extreme abnormal, the finish overall viscosity also can decrease, thus for the mobility of the appropriateness that maintains whole finish provides may.
The present invention comprises C more than at least 10 kinds as the polyether compound of smooth agent
4~ C
18the support of fatty alcohol oxygen ethylene oxide,1,2-epoxyethane isopropyl atactic polyether, block polyether or the random admixtured polyether of block, preferably C
8~ C
12the support of fatty alcohol oxygen ethylene oxide,1,2-epoxyethane isopropyl atactic polyether, block polyether or the random admixtured polyether of block, its single amounts of components all is no more than 10% of pure finish gross mass.Experimental study shows, by single finish component, particularly those are controlled at and account for below 10% of pure finish amount at 30 ~ 90 ℃ of consumptions that the finish component that sticky gentle sticky dense characteristic is abnormal arranged, so, even indivedual finish components may occur being separated when a certain specified temp of experience and concentration, but because shared mass fraction ratio is little, and be unlikely to cause finish integral body that fluctuation is by a relatively large margin arranged on performance.In addition, the polyether compound that is used as smooth agent also comprises 2 ~ 5 kinds of polyether compounds containing ester bond or amido link, as C
4~ C
18aliphatic acid polyoxy ethylene ester and/or its dibasic acid esters and C
12~ C
18fatty acid amide polyoxyethylene ether, specifically be selected from castor oil acid polyoxyethylene ester, oleic acid polyoxyethylene ester, laurate polyoxyethylene ester, two laurate polyoxyethylene dibasic acid esters, castor oil acid acid amides polyoxyethylene ether and oleamide polyoxyethylene ether.These heat decomposition temperatures containing the polyether compound of ester bond and amido link are relative higher.The use amount of polyethers smooth agent accounts for 60 ~ 75% of pure finish gross mass.
In the finish system, the emulsifying agent role is exactly to reduce the surface tension of finish component, increase finish composition activity composition each other and they and water between intermiscibility, stop and occur being separated in the fiber process process.When the finish component occurs that the mass number be separated is larger, the oil slick of separating out needs to remove in time, otherwise can cause the lousiness broken end to increase, and makes the polyester fiber Quality Down.And the removing oil slick has not only increased direct labor's work load, has also improved the finish loss.Polyether compound as emulsifying agent is C
12~ C
18aliphatic acid polyoxy ethylene ester, fatty alcohol polyoxy ethylene ether and/or alkyl phenol polyoxyethylene ether.These polyether compounds specifically are selected from the castor oil acid polyoxyethylene
-x ester, oleic acid polyoxyethylene
-x ester, laurate polyoxyethylene
-x ester, polyoxyethylene nonyl phenyl ethylene
-x ether.Follow " polyoxyethylene " closely and add afterwards " x " expression polyoxyethylene basic weight Complex unit number.Preferably, wherein polyoxyethylene nonyl phenyl ethylene-x ether respectively selects one in x=3 ~ 5 and x=10 ~ 15 liang group, partners; Other polyether compound is selected in x=2 ~ 5 and x=10 ~ 20 liang group compound, is also in most cases respectively to select one to select in pairs.In system, can there be one or more pairs of such emulsifying agents to exist.The HLB value (hydrophilic lipophilic balance) of these polyethers emulsifying agents that the present invention is selected is in two intervals, i.e. HLB=3-6 or HLB=13-18.The compound that the HLB value is 3 ~ 6 can destroy the stability of Water-In-Oil (W/O) type emulsion, and the compound that the HLB value is 13 ~ 18 can destroy the stability of oil-in-water (O/ W) type emulsion.The use amount of polyethers emulsifying agent accounts for 6 ~ 10% of pure finish gross mass.
In adding at a high speed the bullet distortion, polyster fibre will enter the twisting frictional disk by heater.Require finish that suitable frictional behavior is arranged.The too little impact that rubs adds the bullet distortion, and the too great Yi that rubs causes the tension force inequality.Friction between fiber and fiber, fiber and machine part therebetween very easily produces static, because the volume resistance of PET polyester is very high, electric conductivity and hygroscopicity are all very poor, and the electrostatic charge of accumulation is difficult to loss, when accumulation of static electricity just can cause a series of adverse consequences to a certain extent.In the situations such as especially low in humiture, fiber finer, machine operating speed are fast, electrostatic problem is more outstanding, and such as causing that strand disperses, the moulding of silk cylinder is bad, the lousiness broken end, and curlings round the roll etc. need to add antistatic additive for this reason in the finish component.Its antistatic principle, the one, use finish to improve the flatness of fiber surface, fall low-fiber coefficient of friction, thereby also just reduced the static produced because of friction; The 2nd, finish forms thin film at fiber surface, and because moisture absorption and the moisture-retaining capacity of antistatic additive are extremely strong, the moisture in even can absorbed air, form the conduction moisture film at fiber surface, and static is buried in oblivion by conduction in time.In the pfpe molecule structure of antistatic additive, except the hydro carbons group that oleophylic is arranged, hydrophilic strong polar group also must be arranged.The polyether compound antistatic additive that the present invention is used, be to change polyether compound terminal groups R ' into inorganic acid radical, is generally phosphate, sulfuric ester or sulphonic acid ester, or their ester salt; Initial end group R is C
12~ C
18fatty alcohol polyoxy ethylene group or alkyl phenol polyoxyethylene base.The antistatic additive use amount accounts for 4 ~ 7% of pure finish gross mass.The polyether compound antistatic additive is specifically selected is one or more of laruyl alcohol polyoxyethylene sulfuric ester or its ester salt, laruyl alcohol polyoxyethylene phosphate or its ester salt and polyoxyethylene nonyl phenyl ethylene phosphate or its ester salt.At sulfuric ester or its ester salt (O-SO
2-O
-q
+) and phosphate or its ester salt (O-PO (O
-q
+)
2) original preparation form in structure, Q
+=H
+, Li
+, Na
+or K
+, Q wherein
+=H
+mole accounting in sulfuric ester or its ester salt is 0 ~ 80%; And in phosphate or its ester salt Q
+=H
+mole accounting be 50 ~ 90%.When the inorganic salts metal ion consumption of antistatic additive is too much, gently can produce relatively large white powder adding while playing, heavy can coking on hot-rolling, all can cause the fiber lousiness to break end many, affect product quality.
Also be added with the non-polyether type compound that accounts for pure finish gross mass 8 ~ 30% in polyester POY high-speed spin finishes of the present invention, with the function to finish, improve and supplement.These non-polyether type compound additives mainly are used as smooth agent, emulsifying agent, rust inhibitor, oil film reinforcing agent, pH adjusting agent and heat stabilizer etc.
The non-polyether type compound that is used as smooth agent in additive is C
12~ C
18aliphatic acid-C
6~ C
12aliphatic alcohol ester, C
6~ C
12binary of fatty acids-bis-C
6~ C
12fatty alcohol dibasic acid esters, and the low mineral oil of flash-point high viscosity, use amount accounts for 2 ~ 6% of pure finish gross mass.What the non-polyether type smooth agent was specifically selected is oleic acid bay alcohol ester, octyl stearate, di-n-octyl sebacate and dioctyl adipate, and 10
#, 15
#, 18
#, 24
#, 26
#with 32
#one or more of white oil.
The non-polyether type compound that is used as emulsifying agent in additive is C
12~ C
18fatty acid ester, use amount accounts for 2 ~ 8% of pure finish gross mass.What specifically select is one or more of ethylene glycol monolaurate, PGML, propylene glycol mono-oleate, propylene glycol list ricinoleate ester, propylene glycol monostearate, glycerin monostearate and sorbitan monooleate.In these compounds, also have containing ethylene glycol or propylene glycol group, but contained ethylene glycol or propylene glycol group are single, rather than two or more, we list them in the non-polyether type compound.The HLB value (hydrophilic lipophilic balance) of these non-polyether type emulsifying agents, between 3 ~ 6, adds these oiliness non-polyether type emulsifying agents in system, purpose is to regulate the HLB value of whole finish system, the stability of the w/o type emulsion that reduction may occur.
Use because spinning oil is mixed with the aqueous solution, for preventing moisture, corrode the metal surface of relevant mechanical part in process units, need in finish, add relevant rust inhibitor.Use inorganic salts rust inhibitor can increase coking amount, therefore organic compound rust inhibitor is first-selected.Hydrophobic grouping and the polar group that can be adsorbed in metal surface must be arranged in the molecule of organic compound rust inhibitor; the latter is adsorbed in metal surface; even become fine and close chelate sedimentary deposit; and the hydrophobicity alkyl is assembled the formation diaphragm thereon; prevent moisture attack metal surface, play antirust effect.If can in advance or allow the oxide of metal surface become very fine and close in antirust process, rust-proof effect can be better certainly.In addition, also should consider that organic compound rust inhibitor is preferably water miscible.How much relevant the dissolubility of organic molecule in water be with alkyl chain length and hydrophilic polar group.
The non-polyether type compound that is used as rust inhibitor in additive of the present invention is C
12~ C
18fatty acid alcohol ammonium salt, organic dibasic acid alcohol ammonium salt and C
12~ C
18fatty acid hydrazide, use amount accounts for 1.6 ~ 5% of pure finish gross mass.Specifically select be castor oil acid tri ethanol ammonium salt, turkey red oil triethylenetetraminehexaacetic acid alcohol ammonium salt, decanedioic acid tri ethanol ammonium salt, dodecenylsuccinic acid tri ethanol ammonium salt, sulfonation dodecenylsuccinic acid tri ethanol ammonium salt, castor oil acid hydrazides and romote antiquity the oleic acid hydrazides one or more.
In polyester POY-DTY high speed spinning and twisting winding process, between tow and mechanical part, friction increases greatly, particularly at the twisting position, when tow is subject to frictional force, also be subject to the shearing force of spin friction dish, easily cause fibre damage and produce a large amount of white powder.The white powder stickness come off, easily attach on frictional disk, causes the twisting lack of homogeneity, causes dyeing M rate to reduce.White powder mainly is comprised of the polyster fibre crushed products, approximately only has 5% finish to be infected with wherein.If have the component of high film strength in finish, can form very soon homogeneous film protection fiber at fiber surface, reduce abrasion, thereby reduce the generation of white powder, lousiness and broken end.Not only lubricity is good for the two alkyl, polyethers of the low-carbon alcohols end-blocking that the present invention uses in the main part polyether compound of finish etc., also is conducive to increase the film strength of finish at fiber surface.In addition, as additive, also use stearate compounds oil film reinforcing agent, comprised polyether-type stearic acid polyoxy isopropyl support ester and non-polyether type stearic acid C
2~ C
12aliphatic alcohol ester, particularly stearic acid are containing the C of side chain
3~ C
12one or more in aliphatic alcohol ester.Oil film reinforcing agent use amount accounts for 1 ~ 5% of pure finish gross mass.
The non-polyether type compound that is used as pH adjusting agent in additive is selected aliphatic amine and amine oxide thereof, can be expressed as respectively (HOCH
2cH
2)
2rN and (HOCH
2cH
2)
2rN → O, R is C
5~ C
18alkyl or ethoxy, use amount accounts for 0.4 ~ 3% of pure finish gross mass, and amine oxide accounts for 1/10.Finish pH value (10% aqueous emulsion, 25 ℃) is adjusted in 6.5 ~ 7.6 intervals.After adding aliphatic amine and amine oxide thereof, will have the Q of respective numbers in the finish system
+cATION is by Bronsted acid H
+be transformed into RHN
+(CH
2cH
2oH)
2the quaternary ammonium salt ion.
Because polyester POY-DTY technique will be passed through the drawing by high temperature of 190-210 ℃ and add the bullet coiling, require finish used will there is heat endurance preferably, most components of finish can not volatilized in large quantities or decompose in this temperature range.And on the other hand, guarantee again the stable of this temperature range temperature itself, not overheated as far as possible, otherwise just can on hot-rolling, thread guide and hot plate, have many coking materials to generate.The present invention adopts near the additive of boiling point 200 ℃ as heat stabilizer in the design of finish component, and what specifically select is ethylene glycol, and use amount accounts for 1 ~ 3% of pure finish gross mass.197.6 ℃ of ethylene glycol boiling points, have higher heat of gasification (49.6 kJ/mol), and its effect is to prevent that the finish of fiber surface from the drip phenomenon that splashes occurring because of excess Temperature through superheated header the time.Due to molecular weight glycol is less and not with the finish system in unique boiling point lower component--water forms the azeotropic mixture that boiling point is lower, this makes it relatively improve as the efficiency of high temperature finish temperature regulato, is conducive to reduce the amount of being fuming in hot case.
In described method, the water yield added is pure finish, 5 ~ 12% of polyether compound and additive gross mass.
Finish prepared by the inventive method is entering before production line uses, then adds a small amount of preservative agent standby the emulsion that the finish water is converted into 10% left and right simultaneously.
Polyester POY high-speed spin finishes prepared according to the methods of the invention compared with prior art, has following remarkable advantage:
1. between the finish system component, compatibility and resistance to overturning are good.In wire drawing and coiling process process, finish viscosity with temperature and change in concentration are totally more steady, make fiber have good flatness and convergence; In Hou road drafting process, the lousiness broken end reduces, and bar is evenly dry, even dyeing, forming.
2. the finish main body adopts the nonionic surface active agent polyether compound of the many structure types of multicomponent, inorganic content is few, finish emulsion has lower surface tension and better surface-activity, good in thermal property, the not volatile ，Shi Hou road heating cabinet amount of being fuming reduces, and occurs that white powder and coking are few, cleaning frequency is long, and the excellence rate of fibrous finished product significantly improves.
3. finish of the present invention is suitable for large-scale production, product quality and good stability, and low price, cost performance is high.
Below in conjunction with embodiment, the present invention will be further described, but do not form the restriction to right of the present invention.
The specific embodiment
Embodiment 1
The pure finish of active ingredient in oil formula consists of following component and content:
Smooth agent accounts for 76.0% of pure finish gross mass.The polyethers smooth agent has wherein been selected 11 kinds of atactic polyethers, and use amount accounts for 67.4% of pure finish gross mass, and particular compound and consumption thereof are as follows:
In the polyethers smooth agent, castor oil acid polyoxyethylene ester EL20 (2.4%) and block polyether C have also been used
12h
25o (PO)
6(EO)
10h(2.4%).Selected in addition 3 kinds of non-polyether type smooth agents, use amount accounts for 3.8% of pure finish gross mass, and particular compound and consumption thereof are as follows: octyl stearate (1.6%), dioctyl adipate (1.6%) and 18
#white oil (0.6%).
Emulsifying agent accounts for 9.6% of pure finish gross mass, and wherein polyethers is selected the polyoxyethylene nonyl phenyl ethylene
-4 ethers (3.0%) and polyoxyethylene nonyl phenyl ethylene-10 ether (3.0%); Non-polyethers has only been selected ethylene glycol monolaurate (3.6%).
Antistatic additive polyether compound use amount accounts for 4.2% of pure finish gross mass, and what specifically select is laruyl alcohol polyoxyethylene ether-3-sulfuric ester and sodium salt thereof, and both weight ratios of front and back are 1:3.
Rust inhibitor accounts for 4.0% of pure finish gross mass, and what specifically select is turkey red oil triethylenetetraminehexaacetic acid alcohol ammonium salt (1.5%) and decanedioic acid tri ethanol ammonium salt (2.5%); Oil film reinforcing agent use amount accounts for 3.0% of pure finish gross mass, and equivalent is selected stearic acid polyoxy isopropyl support-5 esters and stearic acid isodecyl ester; PH adjusting agent is selected dodecyl diethanol amine and amine oxide thereof, and total consumption accounts for 0.8% of pure finish gross mass, and amine oxide accounts for 1/10; Heat stabilizer ethylene glycol use amount accounts for 2.4% of pure finish gross mass.
Finish preparation first finish main body component press rate of charge by each monomer hold-up vessel through flowmeter accurate-metering vacuum suction reactor, stir and be warming up to 50 ~ 70 ℃, stirring half an hour, then add all the other components and a certain amount of water by formula metering.The water yield added is 11.1% of pure finish gross mass.Stirring is warming up to 70 ~ 80 ℃, maintains 40 ~ 50 minutes, and material in still is put into to airtight filter circulation press filtration to clear, and discharging is to the finished product basin, and product by analysis after the assay was approved, is sent the barrelling of batch mixed still to.The active ingredient 90.0% of finish.
The relevant physical and chemical performance of finish and result of use are referring to table 1 and table 2.
Embodiment 2
The pure finish of active ingredient in oil formula consists of following component and content:
Smooth agent accounts for 73.8% of pure finish gross mass.The polyethers smooth agent has wherein been selected 12 kinds of atactic polyether compounds, and use amount accounts for 62.2% of pure finish gross mass, and particular compound and consumption thereof are as follows:
In the polyethers smooth agent, also be added with oleamide polyoxyethylene ether OAE (3.6%), block polyether L-305 (1.6%) and C
4h
9o (PO)
10[(EO)
10/ (PO)
5] H(1.8%).3 kinds of non-polyether type smooth agents have been selected in addition, oleic acid bay alcohol ester (2.0%), di-n-octyl sebacate (2.0%) and 26
#white oil (0.6%).
The emulsifying agent use amount accounts for 10% of pure finish gross mass, and what wherein polyethers was selected is the laurate polyoxyethylene
-5 esters (3.4%) and laurate polyoxyethylene
-15 esters (3.4%); The non-polyether type emulsifying agent is selected ethylene glycol monolaurate (1.6%) and PGML (1.6%).
That antistatic additive is selected is polyoxyethylene nonyl phenyl ethylene ether-3-PK, C
9h
19c
6h
4o (EO)
3pO
3hK, account for 4.4% of pure finish gross mass.
Rust inhibitor accounts for 4.0% of pure finish gross mass, specifically selects turkey red oil triethylenetetraminehexaacetic acid alcohol ammonium salt (2.0%) and castor oil acid hydrazides (2.0%); What the oil film reinforcing agent was selected is stearic acid isocyanate and isopropyl stearate, and use amount is respectively 1.6%; The total consumption of pH adjusting agent accounts for 2.0% of pure finish gross mass, specifically selects triethanolamine (0.8%) and nonyl diethanol amine and amine oxide (1.2%) thereof, and amine oxide accounts for 1/10; Heat stabilizer is ethylene glycol, use amount 2.6%.
The finish preparation method is with embodiment 1, and the water yield added is 7.8% of pure finish gross mass, and finish active ingredient is 92.8%.The relevant physical and chemical performance of finish and result of use are referring to table 1 and table 2.
Embodiment 3
The pure finish of active ingredient in oil formula consists of following component and content:
Smooth agent accounts for 74.8% of pure finish gross mass.The polyethers smooth agent has wherein been selected 13 kinds of atactic polyether compounds, and use amount accounts for 65.0% of pure finish gross mass, and particular compound and consumption thereof are as follows:
The polyethers smooth agent has also been used two laurate polyoxyethylene-9 dibasic acid esters DLE(2.8%) and block polyether C
8h
17o (PO)
8(EO)
10h(3.0%).3 kinds of non-polyether type smooth agents have been selected in addition: oleic acid bay alcohol ester (1.4%), di-n-octyl sebacate (2.0%) and 15
#white oil (0.6%).
The emulsifying agent use amount accounts for 9.8% of pure finish gross mass, and what wherein polyethers was selected is the castor oil acid polyoxyethylene
-4 esters (3.2%) and castor oil acid polyoxyethylene
-15 esters (3.2%); What the non-polyether type emulsifying agent was selected is propylene glycol list ricinoleate ester (3.4%).
That antistatic additive is selected is laruyl alcohol polyoxyethylene ether-3-PK, C
12h
25o (EO)
3pO
3hK, account for 4.2% of pure finish gross mass.
What in additive, rust inhibitor was specifically selected is castor oil acid tri ethanol ammonium salt (1.8%) and oleic acid hydrazides in romote antiquity (2.0%); What the oil film reinforcing agent was selected is octyl stearate and Ethylhexyl stearate, and use amount is respectively 1.5%; What pH adjusting agent was selected is iso-octyl diethanol amine and amine oxide thereof, and total consumption accounts for 2.2% of pure finish gross mass, and amine oxide accounts for 1/10; Heat stabilizer is ethylene glycol, use amount 2.2%.
The finish preparation method is with embodiment 1, and the water yield added is 5.7% of pure finish gross mass, and finish active ingredient is 94.6%.The relevant physical and chemical performance of finish and result of use are referring to table 1 and table 2.
Proportioning and the resulting polyester POY high-speed spin finishes of finish preparation method quality index according to finish component of the present invention are as follows:
1. the light yellow transparent oily liquid of outward appearance (25 ℃);
2. pH value (10% aqueous emulsion, 25 ℃) 6.5 ~ 7.6;
Viscosity (25 ℃, mPas) 90 ~ 150;
4.10% stability of emulsion (25 ℃), the micro emulsion look transparent or semitransparent, and 72h is breakdown of emulsion not, not wall built-up.
Listed the relevant physical and chemical performance test data of three embodiment finishes of the present invention in table 1.
The physical and chemical performance index of table 1 embodiment of the present invention finish
Listed the result that the relevant performance to adopting three embodiment polyster fibres that finish spins of the present invention is tested in table 2.
Table 2 adopts the performance test data of the polyster fibre that finish spins of the embodiment of the present invention
* 1
* 1draw speed 4600m/min;
* 2central value M=25.0%;
* 3monofilament and multifilament are measured mean value.
Claims (12)
1. the preparation method for the polyester POY high-speed spin finishes, it is characterized in that, by the main body component polyether compound of finish press rate of charge by each hold-up vessel through flowmeter accurate-metering vacuum suction reactor, stirring is warming up to 50 ~ 70 ℃, continue to stir 20 ~ 60 minutes, then add the additive component of finish by formula metering; After adding a certain amount of water, stirring is warming up to 70 ~ 80 ℃, maintains 40 ~ 50 minutes, and material in still is put into to airtight filter circulation press filtration to clear, and discharging is to the finished product basin, and product by analysis after the assay was approved, is sent the mixing kettle barrelling to;
Outside described finish dewaters, pure finish is comprised of main part and additive; Described main part comprises polyether compound more than 20 kinds, accounts for 70 ~ 92% of pure finish gross mass; All the other components are additive, account for pure finish gross mass 8 ~ 30%; In described pure finish, the molecular weight of all components is all below 4000, and wherein 80wt% is between 600 ~ 2800;
Described polyether compound has the molecular structure of following general formula:
RO[(EO)
x/(PO)
?y]R’
Wherein, initial end group R and terminal groups R ' are H, or C
1~ C
18alkyl, aryl, acyl group or amide groups, also or be inorganic acid radical; [(EO)
x/ (PO)
y] be by oxygen ethylene group EO=-CH
2cH
2o-and/or oxygen isopropyl support group PO=-CH
2cHMeO-or-CHMeCH
2the polyether segment that O-forms, x and y are respectively the molal quantity of EO and PO.
2. the preparation method for the polyester POY high-speed spin finishes according to claim 1, is characterized in that, in described polyether compound molecule, contained polyether segment [(EO)
x/ (PO)
y] be pure polyoxyethylene ether chain (EO)
xor polyoxy isopropyl support ether chain (PO)
y, or the random admixtured polyether chain of the atactic polyether chain formed by EO and PO, block polyether chain or block.
3. the preparation method for the polyester POY high-speed spin finishes according to claim 1 and 2, it is characterized in that, described polyether compound comprises smooth agent, emulsifying agent and antistatic additive component, wherein the smooth agent use amount accounts for 60 ~ 75% of pure finish gross mass, the emulsifying agent use amount accounts for 6 ~ 10% of pure finish gross mass, and the antistatic additive use amount accounts for 4 ~ 7% of pure finish gross mass.
4. the preparation method for the polyester POY high-speed spin finishes according to claim 3, is characterized in that, the polyether compound that is used as smooth agent in described polyether compound comprises C more than at least 10 kinds
4~ C
18the support of fatty alcohol oxygen ethylene oxide,1,2-epoxyethane isopropyl atactic polyether, block polyether or the random admixtured polyether of block, also comprise 2 ~ 5 kinds of C
4~ C
18aliphatic acid polyoxy ethylene ester and/or its dibasic acid esters and C
12~ C
18fatty acid amide polyoxyethylene ether.
5. the preparation method for the polyester POY high-speed spin finishes according to claim 4, is characterized in that, the polyether compound that is used as smooth agent in described polyether compound comprises C more than 10 kinds
8~ C
12the support of fatty alcohol oxygen ethylene oxide,1,2-epoxyethane isopropyl atactic polyether, block polyether or the random admixtured polyether of block, its single amounts of components all is no more than 10% of pure finish gross mass; Also comprise that 2 ~ 5 kinds are selected from castor oil acid polyoxyethylene ester, oleic acid polyoxyethylene ester, laurate polyoxyethylene ester, two laurate polyoxyethylene dibasic acid esters, castor oil acid acid amides polyoxyethylene ether and oleamide polyoxyethylene ether.
6. the preparation method for the polyester POY high-speed spin finishes according to claim 3, is characterized in that, the polyether compound that is used as emulsifying agent in described polyether compound is alkyl phenol polyoxyethylene ether, C
12~ C
18fatty alcohol polyoxy ethylene ether and/or C
12~ C
18aliphatic acid polyoxy ethylene ester.
7. the preparation method for the polyester POY high-speed spin finishes according to claim 6, is characterized in that, the polyether compound that is used as emulsifying agent in described polyether compound is selected from the castor oil acid polyoxyethylene
-x ester, oleic acid polyoxyethylene
-x ester, laurate polyoxyethylene
-x ester and/or polyoxyethylene nonyl phenyl ethylene
-x ether.
8. the preparation method for the polyester POY high-speed spin finishes according to claim 3, it is characterized in that, the terminal groups R ' that is used as the polyether compound of antistatic additive in described polyether compound is phosphate, sulfuric ester or sulphonic acid ester, or their ester salt; Initial end group R is C
12~ C
18fatty alcohol polyoxy ethylene group or alkyl phenol polyoxyethylene base.
9. the preparation method for the polyester POY high-speed spin finishes according to claim 8, it is characterized in that, the polyether compound that is used as antistatic additive in described polyether compound is selected from laruyl alcohol polyoxyethylene sulfuric ester, laruyl alcohol polyoxyethylene phosphate or polyoxyethylene nonyl phenyl ethylene phosphate, or one or more of their ester salt.
10. the preparation method for the polyester POY high-speed spin finishes according to claim 1 and 2, it is characterized in that, additive in described finish is the non-polyether type compound, comprises pure finish mass percent 2 ~ 6% smooth agents, 2 ~ 8% emulsifying agents, 1.6 ~ 5% rust inhibitor, 1 ~ 5% oil film reinforcing agent, 0.4 ~ 3%pH conditioning agent and 1 ~ 3% heat stabilizer.
11. the preparation method for the polyester POY high-speed spin finishes according to claim 10, is characterized in that, in described non-polyether type compound additive, smooth agent is selected from C
12~ C
18aliphatic acid-C
6~ C
12aliphatic alcohol ester, C
6~ C
12binary of fatty acids-bis-C
6~ C
12fatty alcohol dibasic acid esters or mineral oil, emulsifying agent is selected from C
12~ C
18fatty acid ester, rust inhibitor is selected from C
12~ C
18fatty acid alcohol ammonium salt, organic dibasic acid alcohol ammonium salt or C
12~ C
18fatty acid hydrazide, the oil film reinforcing agent is selected from stearate, and pH adjusting agent is selected from aliphatic amine or its amine oxide, and molecular structure is expressed as respectively (HOCH
2cH
2)
2rN and (HOCH
2cH
2)
2rN → O, R is C
5~ C
18alkyl or ethoxy, heat stabilizer is selected from ethylene glycol.
12. the preparation method for the polyester POY high-speed spin finishes according to claim 11, it is characterized in that, in described non-polyether type compound additive, smooth agent is selected from oleic acid bay alcohol ester, octyl stearate, di-n-octyl sebacate, dioctyl adipate and 10
#~ 32
#one or more of white oil; Emulsifying agent is selected from one or more of ethylene glycol monolaurate, PGML, propylene glycol mono-oleate, propylene glycol list ricinoleate ester, propylene glycol monostearate, glycerin monostearate and sorbitan monooleate; Rust inhibitor be selected from castor oil acid tri ethanol ammonium salt, turkey red oil triethylenetetraminehexaacetic acid alcohol ammonium salt, decanedioic acid tri ethanol ammonium salt, dodecenylsuccinic acid tri ethanol ammonium salt, sulfonation dodecenylsuccinic acid tri ethanol ammonium salt, castor oil acid hydrazides and romote antiquity the oleic acid hydrazides one or more; The oil film reinforcing agent is selected from stearic acid polyoxy isopropyl support ester, stearic acid C
2~ C
12one or more in aliphatic alcohol ester; The molecular structure of pH adjusting agent is (HOCH
2cH
2)
2rN or (HOCH
2cH
2)
2rN → O, R is C
5~ C
18alkyl or ethoxy.
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Cited By (3)
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| CN106049065A (en) * | 2016-07-08 | 2016-10-26 | 苏州夏尔植物油脂科技有限公司 | Spinning oil for POY (polyester pre-oriented yarn) and preparation method of spinning oil |
| CN109056318A (en) * | 2018-08-15 | 2018-12-21 | 江苏四新界面剂科技有限公司 | Vinegar fibre finish dedicated biomass compound emulsifying agent |
| CN114016292A (en) * | 2021-11-17 | 2022-02-08 | 大连格尔迈斯合成材料有限公司 | Oil agent, filament polyester geotextile and preparation method thereof |
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| CN114016292A (en) * | 2021-11-17 | 2022-02-08 | 大连格尔迈斯合成材料有限公司 | Oil agent, filament polyester geotextile and preparation method thereof |
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|---|---|
| CN103437186B (en) | 2015-07-15 |
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