GB2190098A

GB2190098A - Viscosity regulators for water based spin finishes

Info

Publication number: GB2190098A
Application number: GB08710437A
Authority: GB
Inventors: Force Gunilla E Gillberg-La; Helen A Kravas
Original assignee: Celanese Corp
Current assignee: Celanese Corp
Priority date: 1986-05-05
Filing date: 1987-05-01
Publication date: 1987-11-11
Anticipated expiration: 2007-05-01
Also published as: GB8710437D0; JP2594791B2; DE3714759A1; JPS62276081A; GB2190098B; DE3714759C2

Description

GB 2 190 098 A 1

SPECIFICATION

Viscosity regulators for water-based spin finishes 5 Backgroundof the invention

1. Field of the invention

The present invention relates to finish compositions for yarns and more particularly, to associative thick eners which enable the viscosity of the composition to be controlled as a function of the water content. 10 2. Description of the priorart

Spin finishes and process finishes are compositions normally employed in the fiber industryfor lubrication of filaments oryarns during textile operations i.e., during the melt spinning, drawing, weaving or knitting or otherwise fabricating individual filaments or staple fibers into various textile articles. In addition to the es- 15 sential lubricating agent and its solvent or emulsifying liquid, such as water, small amounts of other modify ing agents may also be present. Generally, finishes comprise a lubricating oil, an antistatic agent, and an emulsifier.

The spin and process finish compositions are generally applied as dilute aqueous solutions having an oil base content by weight in the range of 1 to 30% and preferably 8 to 15%. The viscosity of the composition 20 should be less than about 10 cps to ensure good spreading of the finish on theyarns.

A large number of spin and process finish compositions have been developed overthe years. The com position of such finishes, of course, depends on the specific process requirements. Typically, a key consider ation in formulating suitable compositions is the viscosity of the oil component of the finish since such was observed to influence the number of broken filaments and the tackiness of the snowformed on thetexturings 25 disks. Thus, it has been observed that, in terms of optimizing the composition with respect to the snow formation, the viscosity of the initial oil-based composition ideally should be less than 60 cps at 45'C, while a higherviscosity is needed at intermediate water contents during the processing.

Despite the careful controlling of the viscosity of the oil component or, at most, of the initial water/oil emulsion, the treated yarns have nonetheless not been completely satisfactory but rather, have often exhibi- 30 ted mediocre or poor package build characteristics and poor yarn bundle coherence properties.

Summary and objects of the invention

In view of the foregoing limitations and shortcomings of prior art spin and processing finish compositions as well as other disadvantages not specifically mentioned above, it should be apparentthat there still exists a 35 need in the artfor a finish composition which, in addition to imparting desirable properties to the spun yarns in terms of the number of broken fils as well as the tackiness of the snowformed on the texturings disks, also imparts desirable package build and spin line coherence characteristics. It is therefore a primary objective of the present invention to fulfill that need by providing a spin or process finish composition based on thefact thatwater rapidly evaporates from the finish after its application onto the yarns and that the viscosity of the 40 finish as a function of this observed decrease in the water content markedly affects both the package build and spin line coherence properties of the finish.

More particularly, it is an object of this invention to provide a spin or process finish composition having an associative thickener which does not affect sig nif icantly the viscosity of the initial oi 1-based finish composi tion but which effects a rapid increase in the viscosity of the a ppi ied composition as water evaporates there- 45 from.

Yet another object of this invention is to provide a spin or process finish composition having incorporated therein an associative thickener which enables the viscosity of the spin or process finish to be controlled as a function of its water content so as to optimize the spin or process finish with respect to all of the aforement ioned properties. 50 Another object of this invention is to provide an associative thickener which is miscible with the oil base of the finish and can be diluted into homogeneous watersolutions.

It is a further object of this invention to provide a method of treating spun yarns with the spin or process finish compositions of the present invention containing an associative thickener.

In a first aspect,the present invention provides a spin or processfinish composition comprising; 55 (A) from about 70 to about 99.5% by weight water; and (B) from about 0.5 to about 30% byweight of an oil-based composition comprising:

(i) a lubricating oil in an amount sufficientto achieve the lubrication of a material contacted with the composition; (ii) an emulsifier in an amount sufficieritto emulsify the lubricating oil and water; and 60 (ill) an associative thickener in an amountwhich does not substantially affect the initial viscosity of the spin finish composition yet causes a substantial and rapid increase in the viscosity of the composition asthe water contained therein decreases from its initial level, and has no substantial affect on the viscosity of the composition as the water contained therein decreases to below 40%.

In another aspect, the present invention provides a process for treating yarns with the water-based spin or 65 2 GB 2 190 098 A 2 process finish composition of the present invention containing an associative thickener.

With the foregoing and other objects, advantages, and features of the invention that will become hereinaf ter apparent, the nature of the invention maybe more clearly understood by reference to the following detailed description of the invention, the appended claims and the drawings.

5 Brief description of the drawings

Figure 1 depicts the variation in viscosity as a function of water content of a spin f inish modified with 0.1 % and 0.5% of polyacrylamide.

Figure2 depicts the variation in viscosity as a function of water content of a spin finish modified with 2.5% and 5% of Thickener A. 10 Figure 3 depictsthe variation in viscosity as a function of water content of a spin finish modified with 1 % and 2.5% of Thickener B. Figure 4depictsthe variation in viscosity as a function of water content of a spin finish modified with 2.5% and 5% of Thickener B. Figure 5depicts the variation in viscosity as a function of water content of a spin finish modified with 1 % 15 and 2.5% of Thickener C.

Figure 6depictsthe variation in viscosity as a function of water content of a spin finish modified with 2.5% and 5% of Thickener D.

Figure 7 depicts the variation in viscosity as a function of water content of a spin finish modified with 2.5% and 5% of Thickener E. 20 Figure 8 depicts the variation in viscosity as a function of water content of a spin finish modified with 2.5% and 5% of PLURASAFE 120OR.

Figure 9 depictsthe variation in viscosity as a function of water content of a spin finish modified with 2.5% and 5% of purified PLURASAFE 120OR.

Figure 10 depicts the variation in viscosity as a function of water content of a spin finish modif ied with 2.5% 25 and 5% of Thickener C.

Figure 11 depicts the variation in viscosity as a function of water content of a spin finish modified with 2.5% and 5% of Thickener D.

Detailed description ofpreferredembodiments 30

As a result of the associative thickeners of the invention, finish compositions are produced which exhibit good spreadability when applied to the yarns, exhi bit a rapid and su bstantial initial increase in viscosity as water evaporates from the compositions, and have relatively little affect on the viscosity profile atwater contents less than 40%. Preferably, in orderto obtain good package build, the finish compositions containing the associative thickeners also exhibit a relatively u naffected viscosity profile in the 40-60% by weight water 35 content range.

As mentioned above, previous attempts at formulating finish compositions have generally focussed on the viscosity of the oil base component or, at most, on the viscosity of the initial oil/water emulsion which is applied to the yarns. Such a focus, however, has proven to be unduly narrow since it has been observed that a high degree of evaporation of water and possibly othervolatile components occurs during the application 40 process as well as afterthe spin finish has been applied. Accordingly, the moisture content of the applied spin finish on a freshly spun package may be 50% or even lower depending on the spinning speed i.e., the air flow velocity and its turbulence along the spin line, humidity and temperature at the spin line, yarn bundle configuration (related to surface area); finish distribution on the yarn bundle and, to a certain extent, the finish composition. The water content of process finishes, such as drawframe finishes, depends on the 45 drying conditions.

Sincewater or othervolatile components evaporatefrom thefinish composition during or after its applica tion, an increase in viscosity occurs. The nature of that increase has now been observed to affectthe package build and yarn bundle coherence properties of the spun yarns. More specifically, in orderto obtain good package build and good yarn bundle coherence,the spin finish should exhibit a rather rapid initial viscosity 50 increase aswater evaporatesfrom the composition, such as at least about 100 cps, preferably at leastabout cps as the water content decreasesto about70 to 90% byweight or less. Additionally, the finish composi tion should exhibit a viscosity generally ranging from 150to 600 cps and preferably 200to 400 eps as deter mined by standard techniques (e.g., a Brookfield viscometer) under low or intermediate shearconditions when thewatercontent in the composition is reducedto about 50%. 55 An ideal spin finish therefore should have:

(i) a low viscosity at application concentrations e.g., less than 100 cps, preferably less than 10 cps when the water content is at the initial 70-99.5% level and especially at the 90-99.5% level, to allow a quick spread ing across the yarn bundle; (ii) a rapid viscosity increase upon initial evaporation of waterto 70 to 90% or less of the spin finish to 60 yield good yarn bundle coherence; (iii) an intermediate viscosity of 150 to 600 eps, preferably 200 to 400 cps at water contents of 40-60% by weightto yield good package build; and 0v) a low oil viscosity e.g., less than about 60 cps at 450C. to diminish the number of snow deposites as well as the number of broken f ils attextu ring. 65 3 GB 2 190 098 A 3 As previously indicated, spin finish compositions have typically been prepared by focusing on the prop- erties of the oil component or of the initial oil/water emulsion which is applied. Not surprisingly, the formula tion of a spin finish composition which is ideal in terms of the number of snow deposits, the number of broken filaments at texturing, package build, yarn bundle coherence, and initial spreadability has proven elusive in the art. Thus, one finish was shown to give excellent package build and low snow at texturing but, 5 nevertheless, showed problems with respect to the number of broken fi Is when octaloba I partially oriented yarns were treated. Another spin finish composition showed good broken fil protection but gave heavy snow deposits and poor package build. Yet another composition showed excellent texturing performance but again exhibited poor package build.

In orderto obtain a spin finish composition more closely approximating the ideal compositions described 10 above, it was proposed to incorporate therein standard waterthickeners such as xanthan gum or a polyacrylamide. Although xanthan gum caused a rapid linear increase in viscosity as the water content decreased, water contents less than 50% could not even be examined since xanthan gum gel has a low and slow solubility in water and thus does not perform well as the water contents are decreased to any degree.

The incorporation of 0.1 % byweight of a polyacrylamide viscosity modifier into a conventional spin finish 15 composition was observed to have no initial effect on the viscosity of the composition thus making its use advantageous in terms of spreadability. Additionally, as the water content decreased to 50% by weight, the viscosity of the spin finish composition reached a maximum value of 250 cps as determined by a Brookfield cone-plate micro viscometer with further decreases in the water content resulting in a sharp decrease in the viscosity. 20 Although the 250 cps viscosity levels corresponding to a water content of 50% are desirable in terms of obtaining good package build, it is difficult in practice to control the water contents of the spin finish com positions with such precision. More specifically, the rate atwhich water evaporates from the composition will obviously be a function of thetemperature and humidity of the environment as well as other processing factors. Accordingly, large variations in the percent water in the spin finish compositions can be expected to 25 occur upon application thereof. Ittherefore becomes apparent upon perusal of Figure 1 thatthe poly acrylamides will not suffice as viscosity modifiers since a mere decrease in water content of the spin finish composition from 50% to 40% will result in decrease in the viscosity from about 250 cps to about 100 cps. It will be appreciated that at 100 cps, the spin finish will not impart the desired package build.

Other conventional viscosity modifiers examined exhibited similar behaviourto the polyacrylamides, i.e., 30 poor package build atthe 40-60% water content range. For example, a spin finish containing 5% (based on the oil component) of polyethyllene oxide had a viscosity of about 75 cps at a 60% water content but a viscosity of nearly 500 cps at about a 55% water content. Thus, seasonal variations in temperature and humidity could have drastic effects on the quality of the treated yarns obtained.

The associative thickeners of the present invention are added io conventional spin finish compositions. 35 Such compositions generally comprise:

Water 70to 99.5, preferably 85-92wt.% 40 Added to the water is 30 to 0.5 wt.% of an oil-based component containing on an oil basis:

lubricant 1 to 90, preferably 20-60wt.% emulsifier 5to50, preferably 10-30wt.% 45 anti-static agent 0.5 to 20, preferably 5-10 wt.% other (bacteriacides, antioxidants, etc.) Oto 20, preferably 2-10 wt.% Suitable lubricants include, but are not limited to substances such as palm oil, coconut oil, cottonseed oil, 50 mineral oil, glycerides, polyglycol esters, butyl stearate, octyl stearate, esters of ofeic acid,tri methylol propanelcapryl ic acid esters, 2-methyl-2-propyl propane-1,3- dioldilau rate 2-ethyl-2-butyi-propane 1,3-dioldilaurate, polysiloxanes certain polyethylene oxide polypropylene oxide ajucts and the like.

The lubricant is preferably dispersed in waterwith the aid of an emulsifying agent including surface active organic compounds such as fatty acid salts, higherfatty alcohols, sorbitol esters or sorbitans, phosphate 55 esters, sulfonated aromatic petroleum hydrocarbons, suifonated naphthenates, sulfated vegetable oils, poly oxyethylene esters and ethers, polyglycerol esters, glycerol mono-di- fatty acid esters and the like.

Anti-static agents are added to reduce the electrostatic charge of the f ilament during its subsequent pro cessing. Useful agents include cationic compounds containing a quarternary ammonium-, pyridium-, im idazolinium-, and quinolinium function, and phosphated alcohols, ethyloxated amides and the like. 60 The associative thickeners are present in an amount ranging from about 0. 1 to about 15%, preferablyfrom about 1 to about 5% by weight based on the components of the spin finish exclusive of water, i.e., the oil base.

The associative thickeners must be compatible with the spin finish compositions in that they do not substan tially adversely affectthe beneficial results obtained from the other components of the composition. Gener ally, they are polymeric surfactant-type compounds which act as abridge between droplets in the spin finish 65 4 GB 2 190 098 A 4 emulsion. More specifically, by virtue of a hydrophilic backbone and at least two pendent hydrophobic side chains, the associative thickeners of the present invention, when present above a certain concentration in the water, form associative structures which give viscosity values which are surprisingly high in light of the relatively low molecularweight of the polymers. Without being limited to theory, it is believed that the hydrophobic side chains of the associative thickeners have the capability of competing with surfactants at an 5 emulsion droplet interface. More specifically, the pendant hydrophobic side chains on one molecule interact with the different emulsion droplets or micelles and thereby act to crosslink them. By virtue of the interaction of the associative thickeners, far greater increases in viscosity are observed than would be expected if the viscosity increase were attributable solely to a thickening of the aqueous component.

The amount of a particular associative thickener is selected such that it does not substantially affect the 10 initial viscosity of the spin finish, yet causes a substantial increase in the viscosity of the composition as the water content decreases from its initial level and effects no substantial change in the viscosity as the water content further decreases to below about 40%. In order to obtain good package build, it is additionally des ired to incorporate an amount of associative thickener into the spin finish which wi I I exhibit an intermediate viscosity in the 40-60% by weight water content range. 15 To determine whether a particular associative thickener meets the foregoing criteria, the finish composi tion without the associative thickener is first prepared and its viscosity is determined such as by a Brookfield viscometer. The finish composition is then prepared with the associative thickener present and its viscosity (i.e., the initial viscosity) is again determined. Typically, the viscosity of the spin finish composition with the associative thickener present will increase less than about 20 cps and preferably less than about 10 cps as 20 compared to the composition which does not include the associative thickener.

The water content of the finish composition is then reduced (e.g., by evaporation of the preparation) and the viscosity again determined and compared with the initial viscosity. Typically, as the water content drops to below about 90%, there wil I bean increase in viscosity off rom about 10 to 1000cps.

Awide variety of associative thickeners maybe employed. One associative thickener found suitable forthe 25 present invention is based on copolymers of 1,3-dioxolane and aliphaticl, 2epoxides. These copolymers are described in detail in U.S. Patent No. 4,415,701, the disclosure of which is hereby incorporated by reference.

Specifically, 1,3 dioxolanes of the formula:

0 30 0 wherein R is either hydrogen or Cl-C3 alkyl, are reacted with a C10-C36 monoepoxide of the formulae:

0 35 W- CH2 0 0 W-C-OCH2-Hc- or 40 0 W-CH W.' 11- -CH2 wherein R'iS C7 C33, preferably C9 - C22. Additionally, up to 25% by weight, based on the total monoepoxide 45 weight, of an alkyl or any monoepoxide containing less than about 10 carbon atoms maybe used as a commonomer. Examples of such monoepoxides include butyl glycidyl ether, phenyl glycidyl ether, ethylene oxide, propylene oxide, butylene oxide and the like. 10%byweightof monoepoxide of an aromatic oraliph atic polyepoxide may also be added.

The 1,3 dioxolane monomer may contain up to 10% by weight of trioxane based on the total 1,3 dioxolane 50 weight.

The reaction between the epoxide and dioxolane is catalyzed using well known cationic polymerization catalysts.

Other materials suitablefor use as associative thickeners are the materials described in U.S. Patent Nos.

3,393,157; 4,288,639; 4,302,349 and 4,304,902 as well as the nonionic polymer surfactants described in the 55 article "Nonionic Polymer Surfactants" by C.M. Landoll, Journal of Polymer Science; Polymer Chemistry Edition, Vol. 20, p. 443-455 (1982) the disclosure of which are all incorporated by reference.

Thusjor example, suitable materials include polymers formed from cyclic ethers andlor cyclic acetalsto produce polymeric materials not exclusively composed of oxymethylene groups. Specifically, a cyclic ether having the formula: 60 H_(H Rl-- C -R2)n 1 65 o-i GB 2 190 098 A 5 wherein R, and R2 are each alkyl,cycloalkyi,aryi,alkoxy or aryloxy and n has a value of 1 to 4, or acyclic acetal having one of the following formulae:

5 or a mixture of any of the cyclic ethersand/oracetals among themselves or with acyclic acetal having the formula:

10 is polymerized in the presence of a catalyst consisting Of S03.

Another example of a suitable material is represented by the formula: 15 R[O-(CH2CH20)x- (CH- CH - 0)y- H], 1 1 R' W' 20 whereinzisl or2; Rjorz= 1, is alky], aralkyl, or alkylaryl of 8 - 22 carbon atoms in the alkyl chain, or hydroxyalkyl of 2 -22 carbon atoms, and,forz = 2, is (aryi) alkylene of 4- 18 carbon atoms, R'and Weach independently is hydrogen or Cl - C20 alkyl wherein Wand W' are not simultaneously hydrogen and R'and W' together have 8- 20total carbon atoms, xis 10 -40 andy is 1.2 -5.

The above-described compounds can be prepared by reacting a compound R(O1H1)z in the presence of a 25 basic or acidic catalyst first with ethylene oxide and then with an epoxyalkane of the formula:

W- CH - CH - W' 0 30 A sti 11 f u rther exa m p] e of su ita bl e m ateria 1 s a re co po lym ers of ethyl ene oxide a nd e poxy-n-a 1 ka ne of 12 to carbon atoms. These copolymers contain 96 to 99.9% by weig ht of ethylene oxide and 4 to 0. 1 % by weig ht of th e epoxy-n-al ka ne a n d have a m ol ecu 1 a r wei g ht of betwee n 200,000 a n d 800,000.

The group of associative thickeners disclosed in U.S. Patent No. 4,288, 639 have been found particularly 35 adva ntag eo us for use i n the s pi n f i n ish co m positi o ns of th e present i nve ntio n. They co m prise a 1 p ha-o 1 ef i n oxi de-mod ifi ed 1 iq u id polyeth er thi ckeners wh ich a re obta i n ed by ca p pi ng with a n a 1 p ha-o 1 efi n oxi de, a 1 iq u id stra ig ht-ch a i n po lyoxya 1 kyl ene h eteric or bl ock co polym er i nterm ed iate wh ich is prepa red by reacti ng ethyl ene oxide a n d at 1 east one oth er 1 ower a 1 kylene oxid e havi n g 3 to 4 ca rbon ato m s with a n active hyd rog en contai n i ng a 1 i phatic or a 1 kyla romatic in itiator h avi n g on ly o ne hyd rog e n atom a nd a bo ut 12 to 40 about 18 a 1 i p hatic ca rbo n ato ms.

Altern atively, the thickeners ca n be prepa red by co polym erizi n g a m ixtu re of ethyl e ne oxide a nd th e 1 ower a] kyl ene oxi des i n the p rese nce of th e a 1 ph a-ol efi n oxide. 1 n ad d ition, ethyl ene oxid e homopo lym ers ca pped with the a] pha-o 1 ef i n oxide a re usef u 1. The th ickeners a re sa i d to exh i bit a n u nexpected th icken i n g efficiency in aq u eou s systems as corn pa red with mo re conventio n a 1 po lyeth er th ickeners of th e sa me mol ecu 1 a r 45 weight.

The disclosed use of the thickening agent of U.S. Patent No. 4,288,639 is as a component of water based hydraulicfluids such as that currently marketed under the trademark Plurasafe R, which is registered BASIF Wyandotte Corporation.

The physical properties of a group of associative thickeners employed in the Examples of the invention are 50 setforth in the Table below:

Table 1

Average 55 %Vikolox 1,2-epoxide of molecular Thickener added alkyl chain solution cps weight A 5 C20-24 100 - - B 10 C18 112,000 17,500 60 C 5 C16 16,400 28,000 D 5 C16 950 33,000 E 5 C16 1,400 -- Vikolox is a series of monoepoxide compounds availablefrom Viking Chemical Company. Forexample, 65 6 GB 2 190 098 A 6 Vikolox20-24is a mixture of 47% C20,44% C22and 9%C24carbon-containing monoepoxides having an aver age molecular weight of 313 and a melting pointof 34-40'C.

Thespinfinish composition, including one of the above-described associative thickeners of the reference patents orTable 1, may be applied to the spun yarns by any conventional technique such as byapplyingthe 5 spin finish composition totheyarns immediately afterthe spinning operation by passing theyarnsthrough a trough or having the yarns make contactwith a "kiss" roll rotating in a trough fitted with thespin finish.The spin finish may also be applied by spraying.

The finishes are typically applied to the material atthe rate of 0.01 to 5% and preferably at 0.1 to 1 % by weight of the material. It will be appreciated thatthe amounts are dependent on the processing conditions 10 and are easily ascertained by one of ordinary skill in the art.

The yarns orthe like treated with the modified spin finishes are typicallyformed of polyethyleneterephtha late although the invention may be practiced in conjunction with other materials such as nylon, poly propylene, vinyl acetate, polybenzimidazole and other natural or synthetic f ibers.

The following Examples are given byway of illustration and should not be construed as limiting the subject 15 matter disclosed and claimed.

Example 1

Associative thickener A was incorporated into a spin finish oil base comprising 0.5 parts lubricant, 0.4 parts emulsifiers, 0.02 parts antistatic agents, and 0.002 parts antioxidant. The oil base containing theassociative 20 thickener A was then added tothewater. Specifically, the variation of viscosity as afunction of watercontent wascletermined fora composition containing 2.5%and 5% of associative thickener based on oil.As isevident from Figure2, associative thickener A has no appreciable effectonthe composition's viscosity at highwater contentswhen comparedtothe unmodified finish. However, as water evaporated, an almost immediate difference inviscosity betweenthe modified and unmodified compositionswas observed,with theun- 25 modifiedfinish having a viscosity& lessthan about50cps ata 60% water content whereas the viscosity of the modified composition containing 2.5% and 5% of associative thickener A (based on oil) were about 175 cpsand 350cps respectively. ltwill be appreciated that in thewatercontent range of from 60-40%,the modified compositions neverhad viscosity lowerthan about 175cps in contrasttothe unmodified spinfinish base. Additionally, aswatercontents lowerthan about 40%, the viscosity of the modified compositionsare 30 relatively unaffected.

Example2

The same viscosity/water content relationship determined with respect to associative thickenerA in Ex ample 1 was repeated with associative thickener B at concentrations of 1%, 2.5% and 5% based on the oil 35 content of the same spin f inish described in Example 1.

As is evidentfrom Figures 3 and 4, the modified finishes exhibited far more rapid initial viscosity increases as the water content of the finish decreased than did the unmodified compositions. The modified com positions also exhibited far more desirable viscosity characteristics in the 40-60% water content range and exhibited a substantially unaffected viscosity profile atwater contents lowerthan about 40%. 40 Example 3

The viscosity/water relationship of the spin finish of Example 1 modified with 1 % and 2.5% (on oil) of associative thickener C was determined. As shown in Figure 5, a far sharper, initial increase in viscositywith decreasing water contentwas observed forthe modified spin finishes than with the unmodified spin finishes. 45 Likewise, in the critical 40-60% water content range, the modified spin finishes of the present invention exhibited far more desirable viscosity characteristics. For example, the viscosity of the spin finish containing 2.5% of associative thickener C varied from about 300 cps to about 200 cps in the 40-60% water content range whereas the unmodified f inish varied from less than 50 cps to about 150 cps.

50 Example 4

The same viscosity/water relationship was determined forthe spin f inish of Example 1 modified with 2.5% and 5% (on oil) of associative thickenerD. As Figure 6 demonstrates, there was once again a far greater initial viscosity increase observed with respect to the modified finish than with the unmodified finish. The viscosity of the modified compositions in the 40-60% water content range were likewise superiorto the unmodified 55 spinfinishes.

Example 5

The viscosity/water relationship for the finish of Example 1 modified with 2.5% and 5.0% (an oil) of Thick enerE was determined. Once again, as demonstrated by Figure 7, there was afar greater initial viscosity 60 increase as well as a more desirable viscosity profile in the 40-60% water content range.

Example 6

The viscosity/water relationship for the finish of Example 1 modified with 2.5% and 5% (on oil) of PLURA- SAFE 120OR was determined. As shown in Figure 8, a far more rapid initial viscosity was again observed. 65 7 GB 2 190 098 A 7 Additionally, the finish modified with associative thickeners exhibited especially desirable viscosity characteristics in the 40-60% water content range, with the 5% modified thickener varying in viscosity from under 400 cps to about 200 cps.

Example 7 5

The viscosity/water relationship of the finish of Example 1 modified with a purified PLURASAFE 120OR was determined. A water solution of the PLURASAFE was heated above the cloud point, i.e., the temperature at which the polymeric nonionic surfactant no longerwas water soluble. The solution was kept atthistem perature until good phase separation between a water phase reacts in PLURASAFE and a water solution containing other components was obtained. The PLURASAFE phase was collected, diluted with cold water 10 and the process repeated once more. As Figure 9 demonstrates, higher initial viscosities and more desirable viscosity behaviour in the 40-60% water content range were obtained with the finishes containing the associ ative thickeners.

Example 8 15

The effects of the associative thickeners on the viscosity of a spin f inish oil base corn prising 20 parts water, 42 parts 1 ubricant, 35 parts emulsif ier and 3 parts antistatic agent were determined. Specif ica 1 ly, the spin finish was modified with 2.5% (on oil) of Thickener C and 5% (on oil) of thickener D. As demonstrated by Fig u re 10, higher initial viscosity increases as we] 1 as more desirable viscosity behavior in the 40-60% water content range were obtained with the finishes containing the associative thickeners. 20 Example9

The viscosity/water relationship of a spin finish oil base comprising 77 parts lubricants, 21 parts emulsifiers and 0.4 parts antistatic agent and 0.2 pa rts of antioxidant modified with 2.5% (on oil) of PLU RASAFE 120OR and 5% (on oil) of Thickener D were determined. As shown in Figure 11, the PLU RASAFE modified finish 25 exhibited especially desirable viscosity behaviour. More specifically, in addition to exhibiting a rapid initial viscosity increase, the modified spin finish had a viscosity ranging f rom about 250 to under 400 cps in the 40-60% water content range.

The following Table summarizes the results obtained in the Examples set forth above:

30 Table 11

VISCOSITY(cps) ASSOCIATIVE INITIAL BEHA VIOUR IN 35 SPIN THICKENER VISCOSITY 4060% WA TER FINISH % (ON OIL) INCREA SE CONTENTRANGE Example 1 small 30-150 Example 1 A (2.5%) very rapid 150-200 Example 1 A (5%) very rapid 275-350 40 Example 1 B 0%) moderate 100-250 Example 1 B (2.5%) very rapid 150-425 Examplel B (5%) very rapid 300-1800 Example 1 C (1 %) rapid 125-225 Example 1 C (2.5%) very rapid 200-325 45 Example 1 D (2.5%) moderate 175-200 Example 1 D (5%) very rapid 275-900 Example 1 E (2.5%) very rapid 175-350 Example 1 E (5%) very rapid 300-900 Examplel PLURASAFE 1200 (2.5%) rapid 150-200 50 Example 1 PLURASAFE 1200 (5%) very rapid 200-375 Examplel Purified PLURASAFE 1200 (2.5%) rapid 275-600 Example 1 Purified PLURASAFE 1200 (5%) very rapid 250-700 Example8 small 25-225 Example8 C (2.5%) moderate 100-200 55 Example8 D (5%) rapid 200-325 Example 9 small 50-225 Example9 PLURASAFE 1200 (2.5%) rapid 250-300 Example9 D (5%) very rapid 250-600 60 Thus, the spin finishes containing the associative thickeners exhibited for superior viscosity behaviour in terms of both the initial viscosity increase and the level of the viscosity in the 40-60% water content range.

Althouth not shown in the above Table 11, the associative thickeners additionally did not cause unduly high increases in the viscosity of the initial finish compositions.

Although only preferred embodiments are specifically illustrated and described herein, itwill be apprecia- 65 8 GB 2 190 098 A 8 tedthatmany modifications andvariations ofthe present invention are possible in light of the aboveteachings andwithinthe purviewof the appended claims without departing from the spiritand intended scopeof the invention.

Claims

CLAIMS 5

1. A spin finish composition comprising:

(i) from about 70 to about 99.5 %by weight of water; and 30 to 0.5% by weight of an oil-based component comprising:

(ii) a lubricating oil in an amount sufficientto achieve lubrication of a material contacted with the com- 10 position; (iii) an emulsifier in an amount sufficientto emulsify the lubricating oil and the water; and (iv) an associative thickener in an amount which does not substantially affect the initial viscosity of said spin finish composition, yet causes a substantial increase in the viscosity of the composition as the water contained therein decreases from its initial level and effects no substantial change in viscosity as the water 15 content further decreases to below about40%.

2. The spin finish composition of claim 1 wherein said associative thickener comprises between about 0.1 %and 15% by weight of said composition.

3. The spin finish composition of claim 2 wherein said associative thickener comprises between about 1 and 5% by weight of said composition. 20

4. The spin finish composition of claim 1 wherein said associative thickener comprises a polymeric sur factant having a hydrophilic backbone with at least two pendant hydrophobic side chains.

5. The spin finish composition of claim 4 wherein said thickeners are based on copolymers of 1,3 dioxolane and aliphatic 1,2 epoxides.

6. The spin finish composition of claim 1 wherein said lubricating oil comprises between about land 25 about 90% byweight of said oil-based component.

7. The spin finish composition of claim 1 wherein said lubricating oil comprises between about 20 and about 60% by weight of said oil-based component.

8. The spin finish composition of claim 4 wherein said thickener comprises an ethylene oxidelpropylene oxide copolymer end-capped at both ends with twelve to eighteen carbon atom ether linkages. 30

9. The spin finish composition of claim 1 further comprising between about 0.5 to about 20% by weight of an antistatic agent.

10. The spin finish composition of claim 9 further comprising between 5 and about 10% by weight of an anti-static agent.

11. The spin finish composition of claim 1 wherein said emulsifier comprises between about 5 and about 35 50% by weight of said oil-based component.

12. The spin finish composition of claim 11 wherein said emulsifier comprises between about 10 and about 30% byweight of said oil-based component.

13. The spin finish composition of claim 1 wherein said lubricating oil is palm oil, coconut oil, cottonseed oil, mineral oil, glycerides, polyglycol esters, butyl stearate, octyl stearate, esters of oleic acid, trimethylol propane/caprylic acid esters, 2-methyi-2-propyipropane-1,3dioldilau rate, a polysiloxane, a poly ethylene oxide polypropylene oxide adductor mixtures thereof.

14. The spin finish composition of claim 1 wherein said emulsifier is a fatty acid salt, a higherfatty alcohol, a sorbitai ester orsorbitan, a phosphate ester, a sulfonated aromatic petroleum hydrocarbon, a sulfonated naphthenate, a sulfonated vegetable oil, a polyoxyethylene ester or ether, a polyglycerol ester, a 45 glycerol mono-di-fatty acid ester or mixtures thereof.

15. The spin finish composition of claim 1 wherein said associate thickener is the reaction product of 1,3-dioxolane and an aliphatic 1,2-epoxide.

16. The spin finish composition of claim 1 wherein said associative thickener causes less than a 20 cps increase in the initial viscosity of said spin finish. 50

17. The spin finish composition of claim 16 wherein said associative thickener causes less than a 10 cps increase in the initial viscosity of said spin finish.

18. The spin finish composition of claim 1 wherein the viscosity of said composition increases by at least about 100 cps as the water content decreases to between about 70 and about 90% byweight.

19. The spin finish composition of claim 18 wherein the viscosity of said composition increases by at least 55 about 150 cps as the water content decreases to between about 70 and about 90% by weight.

20. The spin finish composition of claim 1 wherein the initial viscosity of said composition is below about cps.

21. The spin finish composition of claim 20 wherein the initial viscosity of said composition is below about20cps. 60

22.The spin finish composition of claim 20 wherein said oil-based component has a viscosity less than about 60 cps.

Printed for Her Majesty's Stationery Office by Croydon Printing Company (L1 K) Ltd,9187, D8991685.

Published bVThe Patent Office, 25 Southampton Buildings, London WC2A l AY, from which copies may be obtained.