US3813338A

US3813338A - Textile-machinery lubricant composition

Info

Publication number: US3813338A
Application number: US00240806A
Authority: US
Inventors: W Coppock; J Amaroso; J Griffith
Original assignee: Sun Oil Co
Current assignee: Sunoco Inc
Priority date: 1970-05-06
Filing date: 1972-04-04
Publication date: 1974-05-28
Anticipated expiration: 1991-05-28

Abstract

AN IMPROVED HIGH RETENTION LUBRICANT FOR TEXTILE-MACHINERY COMPRISES A NAPHTHENIC BASE OIL, A TACKINESS AGENT (E.G., POLYISOBUTYLENE), AND AN EFFECTIVE AMOUNT OF A LITHIUM SOAP (E.G. 0.1-1.5% LITHIUM STEARATE) TO PROVIDE A MECMICHAEL VISCOSITY AT 70* F. OF AT LEAST 15 (PREFERABLY 20-35). THE BASE OIL CAN HAVE A VISCOSITY IN THE RANGE OF 60-600 SUS AT 100* F. (MORE PREFERABLY 125300 SUS) AND AN ANILINE POINT IN THE RANGE OF 150-170* F., SAID BASE OIL COMPRISING AT LEAST ONE HYDROREFINED NAPHTHENIC OIL COMPONENT HAVING A VISCOSITY IN THE RANGE OF 40-12,000 SUS AT 100* F., AND PREFERABLY, IS A WIDE BOILING RANGE BLEND CONTAINING AT LEAST TWO SUCH HYDROREFINED NAPHTHENIC OILS. FOR EXAMPLE, THE LUBRICANT CAN COMPRISE 75 PARTS BY WEIGHT OF 100 SUS HYDROREFINED NAPHTHENIC OIL, 20 PARTS OF 2400 SUS HYDROREFINED NAPHTHENIC OIL, 2 PARTS OF A HIGH MOLECULAR WEIGHT (APPARENT M.W. IN OIL OF ABOUT 100,000) POLYISOBUTYLENE TACKINESS AGENT, 1 PART OF LITHIUM STEARATE, 1.5 PARTS OF CHLORINATED PARAFFIN AS AN ANTIWEAR AGENT, AND 5 P.P.M. OF SILICONE ANTIFOAM.

Description

United States Patent U.S. Cl. 252--42.1 13 Claims ABSTRACT OF THE DISCLOSURE An improved high retention lubricant for textile-machinery comprises a naphthenic base oil, a tackiness agent (e.g., polyisobutylene), and an eifective amount of a lithium soap (e.g. 0.l1.5% lithium stearate) to provide a MacMichael viscosity at 70 F. of at least 15 (preferably 20-35). The base oil can have a viscosity in' the range of 60-600 SUS at 100 F. (more preferably 125- 300 SUS) and an aniline point in the range of ISO-170 F., said base oil comprising at least one hydrorefined naphthenic oil component having a viscosity in the range of 40-12,000 SUS at 100 F., and preferably, is a wide boiling range blend containing at least two such hydrorefined naphthenic oils. For example, the lubricant can comprise 75 parts by weight of 100 SUS hydrorefined naphthenic oil, 20 parts of 2400 SUS hydrorefined napththenic oil, 2 parts of a high molecular weight (apparent M.W. in oil of about 100,000) polyisobutylene tackiness agent, 1 part of lithium stearate, 1.5 parts of chlorinated paraffin as an anti-wear agent, and p.p.m. of silicone antifoam.

CROSS REFERENCE TO RELATED APPLICATIONS The present application is a continuation-in-part of application Ser. No. 35,231, filed May 6, 1970; Ser. No. 60,642, filed Aug. 3,-1970 (now abandoned); Ser. No. 178,193, filed Sept. 7, 1971, and Ser. No. 178,479, filed Sept. 7, 1971.

The following patents and applications are related to the disclosure of the present application in that they disclose additives which are useful in the present composition and/ or methods of obtaining hydrorefined naphthenic oils (and other oils) which can be used to make the textile machinery lubricant oil composition of the present invention.

The disclosure of all of the following applications and patents is hereby incorporated in the present application:

Serial 2 Filing Patent No. date No.

Issue date 730,999- 5-22-68 Pending A.U. 116

(COPA Appeal PA 9011) 3,813,338 Patented May 28, 1974 TABLE-Continued Serial Filing Patent Issue No date No. date Title 812,516. 2-19-69 3, 619, 414 11-9-71 Catalytic Hydrofinishing of Petroleum Distillates in the Lubricating Oil Boiling Range-Ivor W. Mills, Merritt C. Kirk, Jr. and Albert '1. Olenzak.

850,716. 8-18-69 Now abandoned.... Blended Hydrocarbon Oil and Process of ManufactureIvor W. Mills and Glenn R. Dimeler. Now abandoned. Hydrcrefined Lube Oil and Process of Manufacture- Ivor W. Mills and Glenn R. Dimeler. 4-4-72 Process for Preparing High Viscosity Hydrorefined Cable Oil-Ivor W. Mills, Glenn R. Dimeler, William A. Atkinson and David A. Hofiman. Pending A.U. 116.-- Oil and Process of Manuiacture oi Blended Hydrorefined Oil-Ivor W. Mills and Glenn R. Dimeler.

3, 706, 653 12-19-72 Light-colored Highly Aromatic Oil and Process of Preparation-Ivor W. Mills, Glenn R. Dimeler and Merritt C. Kirk, .Tr.

8-1-72 Hydroreflned Cable Oil and Process of Manufacture- Ivor W. Mills and Glenn R. Dimeler.

9-26-72 Hydraulic Oil CompositionJohn Q. Griffith, III, Edward S. Williams grid William H. Reiland,

Pending A.U. Hydraulic Oil Composition Containing a Blended Base Stock-John Q. Gn'flith, III, Edward S. Williams, William H. Reiland, Jr., Ivor W. Mills and Glenn R. Dimeler.

a High Viscosity Index Gary L. Driscoll, Irl N.

Duling and David S.

Olenzak.

Pending A.U. 117... Mist Lubricant Containing Polymeric Additive- James R. Amaroso, Walter J. Coppock, Thomas D. Newingham and Edward S. Williams.

Pending A.U. 117... Composition Comprising Stabilized Hydrocracked Lube and an Antioxidant- Robert B. Bryer, William W. Grouse, Jr., John Q. Griflith, III, Thomas D. N ewingham and William H. Reiland, Jr.

Pending A.U. 165... Soap Thickened Hydraulic Oil Composition-John Q. Griffith, III, Edward S. Williams and William H. Reiland, Jr.

Pending A.U. 161-.. Hydrogenated Ethylene- Propylene Copolymer Oils-Richard S. Stearns, Irl N. Duling and David S. Gates.

Pending A.U. 116..- Hydrorefined Lube Oil and Process of Manufacture- Ivor W. Mills and Glenn R. Dimeler.

Pending A.U. 116-.- Polyisobutylene Oil Having 1 Abandoned Aug. 12, 1972 in favor of the present application.

BACKGROUND OF THE INVENTION A textile-machine lubricant must perform satisfactorily in textile-mill service where adequate lubricating properties must be combined with high retention (e.g., the ability to stay put in a bearing). Stray oil thrown from a bearing can find its way to the cloth being manufactured and complicate the cleaning steps taken at the end of the process.

Prior art textile-machinery lubricants have been compounded with high viscosity index oils (e.g., solvent-refined paraffinic lube oil) and a combination of additives to give the necessary retention properties. One of these materials, a lithium soap, was finely dispersed in the paraffinic oil, but was not in complete solution. Under field conditions, the soap separated from the product. This problem of gel stability has been frequently mentioned in the prior art.

The present invention relates to an improved high retention lubricant for textile-machinery which does not separate under field conditions, and which is equivalent or superior to prior art textile-machinery which does not separate under field conditions, and which is equivalent or superior to prior art textile lubricants in such performance characteristics as lubricating, retention and cloth scourability and which does not discolor or degrade textile fibers.

This improved high retention lubricant is not only resistant to separation but also has brighter appearance, produces less staining if it comes into contact with fabric, and provides rubber seal protection and conditioning. Furthermore, in mill trials this new lubricant provided lower mill consumption of electrical power required by such textile-machinery as Draper Shuttleless Looms.

Among the relevant prior art are the following:

0.8. Pat. No. Patentee Glass/Sub a, et al. Stevens, et al Trent-mam, et al McCarthy, et al 8/58 Brunstrum, at. al 252 41 Donaldson, et al 208/217 X Coppock 252/36 SUMMARY OF THE INVENTION An improved high retention lubricant for textile-machinery comprises a naphthenic base oil, a tackiness agent (e.g., polyisobutylene, isotactic polypropylene, polyacrylates, etc.), and an effective amount of a lithium soap (e.g., 0.1-1.5 lithium stearate) to provide a MacMichael viscosity at 70 F. of at least 15 (preferably 20-35). The base oil can have a viscosity in the range of 60-600 SUS at 100 F. (more preferably 125-300 SUS) and an aniline point in the range of 150-170 F., said base oil comprising at least one hydrorefined naphthenic oil component having a viscosity in the range of 40-12,000 SUS at 100 F., and preferably, is a wide boiling range blend containing at least two such hydrorefined naphthenic oils. For example, the lubricant can comprise 75 parts by weight of 100 SUS hydrorefined naphthenic oil, 20 parts of 2400 SUS hydrorefined naphthenic oil, 2 parts of a high molecular weight (apparent M.W. in oil of about 100,000) polyisobutylene tackiness agent, 1 part of lithium stearate, 1.5 parts of chlorinated paraflin as an antiwear agent, and p.p.m. of silicone antifoam.

The improved high retention lubricant for textilemachinery of the present invention comprises additives and a base oil having an SUS viscosity in the range of 60-600 at 100 F. (more preferably 125-300" R), consisting essentially of one or more hydrorefined naphthenic I oils of the lubricating oil viscosity range (e.g., 45-12,000

SUS at F.) and having an aniline point in the range of -190" F., more preferred -170 F., a viscositygravity constant (VGC) in the range of 0820-0899, more preferred 0840-0899, and an ultraviolet absorptivity (i.e. UVA) at 260 millimicrons, (i.e., 260 UVA) which is at least 40% less than that of an unhydrorefined naphthenic lube of the same viscosity (VGC) and boiling range. Preferably, the UVA of the base oil at 335 millimicrons (i.e., 335 UVA) is in the range of 0.0 to 0.4 (typically 002-02) and the ASTM D1500 initial color is less than 4.0 (more preferably no greater than 2.5).

The additives comprise a tackiness agent and a lithium soap in sufficient quantity to thicken the base oil and provide a minimum MacMichael viscosity, at 70 F., of 15 (more preferably in the range of 20-35, typically about 25). The preferred tackiness agents are olefin polymers (e.g., atactic polypropylene, or polyisobutylene rubber) and can be partially or fully hydrogenated; however, any oil-compatible tackiness agent (e.-g., polyacrylates, Al oleate, or natural rubber obtained from dehydrated latex) can be used. The preferred range for the polyisobutylene polymers as commercially available, as in dilution with oil (about 50%) is 0.3-6%, more preferably l-3%. In any event, the amount used must be sufiicient to cause the lubricant to be highly retentive on a bearing; however, the amount must be less than that which will cause the lubricant to be stringy.

Another preferred additive is an antiwear agent which will not harm textiles, most preferred is 03-10% of a chlorinated parafiin; however, 0.22% of tricresyl phosphate or a combination of these two additives can also be used. Optionally, the improved high retention lubricant for textile machinery can also contain an antifoam (such as 05-20 p.p.m. of active silicone antifoam). Generally such antifoam is used as a dilute solution or suspension containing about 1% of the active ingredient.

To further safeguard against discoloration, an antioxidant such as 0.05-l% ditertiarybutyl paracresol (i.e., DBPC) can also be included.

In general, any additive used in the textile-machine lubricant of the present invention should have an acid number less than 25 and the total, compounded lubricant should have an acid number less than 0.5 and a neutral pH (preferably, 6.2-7.7, more preferred 6.8-7.2).

FURTHER DESCRIPTION The base oil can consist essentially of a narrow-boiling range, hydrorefined naphthenic lube of the desired SUS viscosity or the desired viscosity base oil can be obtained from a Wider boiling range blend of two or more narrowboiling range naphthenic oils (e.g., a 150 SUS base oil can be obtained directly by hydrogenation of a SUS distillate or can be obtained by hydrogenating a blend of 100 and 2500 SUS distillate or, more preferred, the 150 SUS base oil can be obtained by blending a 100 SUS hydrorefined distillate with a 2500 SUS hydrorefined distillate). Processes for obtaining such distillates and such hydrogenated oils are disclosed, for example, in the previously referred to applications and patents of Mills and co-inventors. Such oils are available under the trade name Sunthene.

Although the base oil can have a viscosity at 100 F. in the range of 60-600 SUS, the preferred viscosity range is 125-30 SUS and, more preferred, 140-220 SUS. When the viscosity of the base oil is less than about 125 SUS, the flash point becomes so low that it is difficult to heat the oil sufliciently to incorporate the lithium stearate. Generally the oil should be heated to about 400 F. for proper lithium stearate incorporation.

A blended base stock can be advantageous in such additive incorporation since the lithium can be first incorporated in a hot, higher flash point component oil (e.g., 2500 SUS) and the mixture cooled prior to incorporation of other additives and the lower flash point remainder of the base oil. This flash point problem was considerably less in making prior art textile lubricants with parafiinic base oils since the parafiinic oils have generally much higher flash points for a given viscosity at 100 F. than do hydrogenated naphthenic oils. For lubrication of looms, and most other textile machinery, the viscosity of the base oil at 100 F. is preferably no greater than 300 SUS because a higher viscosity base oil can produce a textile lubricant which causes too great an increase in start-up torque of the machinery. However, a protective coating for metals (e.g., firearms) can be made from the same additives as the textile machinery lubricant and in which the base oil has a viscosity as high as 600 SUS at 100 F.

To improve such properties as color, flash point and oxidation stability, the base oil can also contain in the range of 05-15% of hydrorefined paraffinic oil, solvent-refined parafiinic oil (see Ser. No. 178,193), naphthenic distillate, naphthenic-acid free naphthenic distillate, polyolefin oils or hydrogenated polyolefin oils.

The base oils preferably contain less than 80 p.p.m. of basic nitrogen, more preferably less than 30 p.p.m. (in some cases (0-10 p.p.m.), and can be those described in the previously cited applications of Mills et a1. and, more preferably, are blends of two or more hydrorefined naphthenic oils (e.g., a 150 SUS blend of a 100 SUS at 100 F. hydrorefined naphthenic oil and a 2500 SUS at 100 F. hydrorefined oil) or a blend of hydrorefined naphthenic oil and hydrocracked paraffinic oil.

In the lubricant of the present invention, the base oil can have an aniline point in the range of 140-180, preferably the aniline point of the base oil is in the range of ISO-170 "F. to enable maintenance of good rubber seal condition. Preferably, the oil or blend of oils is selected so as to obtain a base with the desired viscosity, an ultraviolet absorptivity at 335 millimicrons (i.e. 335 UVA) in the range of 001-04, more preferred 002-02, and an aniline point in the range of 150-170" F. The hydrorefined naphthenic oil component of such a base stock will generally have an aniline point in the range of 140- 190, more preferred ISO-170 F.

Lubricants which are mostly paratfinic in structure have high aniline points and will shrink the rubber and make it hard. This permits the lubricant to leak. On the other hand, if the aniline points is below 150 F., excessive swell often occurs and the seal may be cut and torn by the rubbing surface, thereby allowing lubricant to bypass. Seal conditioning additives can also be used to improve seal performance in the lubricant.

The phrases severe hydrorefining or hydrogenation refer to processes conducted in the presence of a hydrogenation catalyst at from about 500-775" F., with hydrogen of 50-100% purity, and from 800-3000 p.s.i. of hydrogen at the reactor inlet (at total pressures from 800- 6000 p.s.i.g.) at a fresh feed liquid hourly space velocity (LHSV) of from 0.1-8.0 (usually below 2.0), preferably conducted either in vapor phase or trickle phase. Such hydrogenation or severe hydrorefining is to be distinguished from hydrocracking in that the production of overhead (i.e., hydrocarbons boiling below 485 F.) is less than 25% by volume per pass through the reactor (and, typically, less than Product recycle, for example, as in US. Pat. 2,900,433, can be used to increase severity. Recycle liquid hourly space velocity can vary from 0 to 20; however, it is preferred to operate at total liquid throughputs that obtain at greater than 25% of flooding velocity and more preferably at from 40-98% of flooding velocity.

Preferably, the temperature is below that at which substantial cracking occurs, that is, no more than 20 weight percent (preferably less than 10%) of the feed stock is converted to material boiling below 300 F. in a single pass through the reactor. Although the maximum hydrogenation temperature which will not produce substantial cracking is somewhat dependent upon the space velocity, the type of catalyst and the pressure, generally it is below 750 F. but can be as high as 785 F. To allow a margin of safety, it is preferred to operate below 700 F. (except when it is desired to obtain a hydrogenated oil containing more gel aromatics than are in the charge). At total pressures below about 2000 p.s.i. the preferred temperature is below about 660 F., since above that temperature the degradation of oil viscosity can become large.

Typical of such severe hydrorefining methods, when conducted within the aforementioned processing conditions, are those of US. Pat. Nos. 2,968,614; 3,993,855; 3,012,963; 3,114,701; 3,144,404; 3,278,420 and 3,642 and those of the previously referred to copending applications, Ser. No. 622,398; 652,026; 636,493; 730,999 and 812,516. The terms severely hydrorefined oil or hydrogenated oil include the products, within the lubricating oil boiling range, of such severe hydrorefining or hydrogenation. One characteristic of a severely hydrorefined or hydrogenated oil is that the ratio of monocyclic aromatics to polycyclic aromatics is significantly greater than in hydrotreated oils or conventional distillate oils.

Where the desired hydrorefined oils is to be of the naphthenic class, a preferred charge to the hydrogenation reactor can be obtained by vacuum distillation of naphthenic or mildly aromatic crude oils (as in US. Pat. No. 3,184,396), especially those crude oils wherein the 1500-3000 SUS (at F.) distillate fractions have viscosity-gravity constants from 0.84 to 0.92. Preferably, such as charge stock should be substantially free of naphthenic acids prior to the hydrorefining (thus, in some cases distillation in the presence of caustic is advantageous). Usually materials boiling below about 600 F. (including residual H S, NH etc.) are removed from the hydrorefined oils, as by atmospheric distillation (and the viscosity can also be adjusted by choice of distillation end point) prior to clay contacting (if the oils are to be clay finished). Such naphthenic distillate oils are available commercially under the trade name Circosol.

The viscosity of the base oil, or of the final hydrorefined oil, can be adjusted by the addition of other oils of higher or lower viscosity and which are within the lube oil boiling range. Where desired, the basic nitrogen content can be lowered by contacting the charge or hydrogenated oil or the blend of hydrogenated oils with suflicient acidic adsorbent or mineral acid to reduce the basic nitrogen content of the oil, as to below 10 p.p.m.

By naphthenic distillate, we refer to a distillate fraction (or a mildly acid treated distillate fraction, or a solvent rafiinate fraction or an acid-treated rafiinate) usually from vacuum distillation, or a crude which is classified as naphthenic (including relatively naphthenic) by the viscosity-gravity constant (VGC) classification method. (See p. 79-80 Plasticizer Technology, vol. 1, p. 5, Bruins, Reinhold Publishing Corp., N.Y., 1965.) Preferably, such crudes are Grade A (wax-free), typically Gulf Coastal, and include, for example, Refugio, Mirando, and Black Bayou. The lower VGC oils can be obtained from midcontinental crudes; and can be dewaxed if desired (as by extraction or isomerization). Such naphthenic fractions will have a VGC in the range of 0.820 to 0.899 and, typically, a viscosity in the range of ISO-12,000 SUS at 100 F. (for example, 500-6000). In some cases the crude (and distillate) can have a VGC as high as 0.94 (such crudes are characterized as mildly aromatic), or higher (e.g., 096+). Deep furfural extraction (e.g., about 50% yield) of a high VGC Grade A crude can be used to produce a wax-free, lower VGC fraction (e.g., 0.83 VGC).

Typically, paraffinic oils are those having a viscositygravity constant (VGC) in the range of 0.790 to 0.819 (preferably above 0.799). Typical of solvent refined paraffinic lubes are those available commercially under the trade name Sunpar. Typical hydrorefined paraflinic lubes are those available commercially under the trade name Sunpar, H series (e.g., Sunpar' llOH).

Naphthenic oils have a VGC in the range of 0.820 to 0.899 and the preferred hydrorefined naphthenic oils have a VGC in the range of 0.850 to 0.899. Hydrorefined, relatively aromatic oils, having a VGC in the range of 0.900 to 0.920, can sometimes be used as a whole or partial substitute for the hydrorefined naphthenic lube. Aromatic oils (including hydrorefined or hydroaromatized oils) having a VGC in the range of 0.921 to 1.050 and greater, canbe useful in minor proportions (e.g., 1-20%) for adjusting the aniline point of the base oil, particularly when the base oil contains a high proportion (e.g., 20%) of a high VI hydrocracked paraflinic oil.

As an additional component to the hydrorefined naphthenic oils previously described, the lubricant can contain a hydrogenated polyolefin oil (e.g., see Ser. No. 220,362 of Stearns et al.; Ser. No. 52,301 of Driscoll et al.; Canadian Pat. 842,290; and U5. Pat. 3,598,740) or a high viscosity index, hydrocracked oil or a mixture of such components. (Such oils can be dewaxed, if desired). In such blends an aromatic oil or concentrate rich in aromatic hydrocarbons (e.g., cycle oil) may have to be added to obtain the proper aniline point for seal swelling.

The preferred polyolefin oils are polymers or copolymers of C -C olefin which have a pour point no greater than --35 F., and preferably below 50 F. The hydrogenation can be from 50% to 100% of saturation and, preferably, is to a bromine number no greater than 10, more preferably less than 5, Preferred polyolefins include ethylene-propylene copolymer, polypropylene, polybutene (especially polyisobutylene), and poly(1-octene).

The high VI hydrocracked parafiinic oil component can be obtained by hydrocraclring a high viscosity distillate or dewaxed distillate from a parafiinic crude (such as Lagomedio) and typically has a VI in the range of 90-105 and contains in the range of 330% of aromatics by clay-gel analysis. The hydrocracked lubes are preferably stabilized (against UV light degradation and sludging) by extraction of the hydrocracked oil with aromatic selective solvents, such as furfural or phenol or by hydrorefining to reduce the 260 UVA at least 30% (preferably 40% For examples of such oils see Ser. No. 178,193 of Bryer et al.

' and US. Pat. 3,579,435 to Olenzak et al.

The preferred stabilized hydrocracked oils (whether extracted or hydrorefined) are characterized by having a D-943 test life (to an increase in acid number of 2.0) which is at least 20% lower than the D-943 life of an unstabilized hydrocracked oil but which is at least 20% greater than the D-943 life (with the usual amount of inhibitor, e.g., 0.5% DBPC) of an unhydrocracked solvent refined parafiinic lube of the same viscosity.

The preferred soap is lithium stearate; however, any of the prior art lithium soaps which have been used in petroleum lubricants can be useful in textile oils of the present invention. Such soaps are shown, for example, in U.S. Pats. 2,489,300 and 3,383,312. For soap thickening, the preferred lithium soaps include soaps of fatty acids containing in the range of 12-22 carbon atoms, preferably an unsubstituted fatty acid. Stearates, palmitates, tallates, laurates, oleates and mixed soaps are among the useful soaps.

ILLUSTRATIVE EXAMPLES In the following examples, as elsewhere in this application, UVA stands for ultraviolet absorptivity, all percentages are by weight and all viscosities are at 100 F., unless otherwise noted.

Example I A high retention, textile machinery lubricant was com pounded using a base oil comprising hydrogenated naphthenic oil, and containing high molecular weight polyisobutylene (as a tackiness agent) and lithium stearate.

The textile machinery lubricant composition had a MacMichael viscosity of about 25 at 70 F. and contained at 150 SUS (at 100 F.) base Oil having an aniline 8 point of 1 62 and consisting of 19.30 parts of 2400 SUS (at 100 F.) hydrorefined naphthenic oil containing 45% aromatics and having a 260 UVA of 5.7 and a 335 UVA of 0.22 and 76.38 parts of 100 SUS (at 100 F.) hydrorefined naphthenic oil containing 35% aromatics and having a 260 UVA of 2.3 and a 335 UVA of 0.03. Both hy-j drorefined naphthenic oils were obtained from naphthenic acid-free, naphthenic distillate by hydrogenation at 625 F., 1200 p.s.i.g. of hydrogen, 0.2 LHSV with a presulfided Ni-Mo-oxide catalyst. Before hydrorelining the SUS distillate had a 260 UVA of 7.3, a 335 UVA of 0.23 and contained 44% aromatics; whereas, the 2500 SUS distillate had a 260 UVA of 10.5, and 335 UVA of 0.68 and contained 47% aromatics.

In addition to the base oil, the textile-machinery oil contained 1.9 parts of commercial polyisobutylene (available under the trade name Partac-N of Enjay Company), 0.7 parts Li stearate, 0.4 parts of DBPC antioxidant, 0.02 parts of a defoamer containing 1% active ingredients (Dow Corning Silicone), and 1.3 parts of chlorinated paraffin (Chlorafin 40), containing 40% chlorine. The chlorinated parafiin imparts especially useful antiwear properties and does not discolor or damage textiles. The degree of chlorination of this additive can vary considerably, depending on the manufacturer and grade; however, all such presently commercially available light colored, chlorinated paraffins can be used in the lubricant of the present invention.

The compounding procedure follows:

Compounding procedure:

1. Mix all of the Li-stearate with all of the 2500 SUS oil and heat to 400-410 F. for 10 minutes with mechanical agitation.

2. Stop heat and add 100 SUS oil-cool as quickly as possible, to about 150 F.

3. Add remaining additives at l40-150 F.

4. Continue agitation until blend cools to 130 F.

Example 2 A textile-machinery lubricant was compounded using the same additives and procedures as that of Example 1, except that the base oil was a 150 SUS solvent refined parafiinc lube (sold as Sunpar having a VGC .of 0.803, viscosity at 210 F. of about 43.6 SUS and an aniline point of 221. The paraflinic lube was made by blending two commercially available solvent refined paratiinic distillates, Sunpar 110 (75.55 parts) and Sunpar (20.00 parts).

Example 3 Another lab evaluation was conducted in a complete Alemite lubrication system. In this study the lubricator was pulsed on 3-minute cycles or about 16 times faster than normal in plant operation. Each lubricant was run for 700 hours, which would be equivalent to about 11,000 hours in the field. Moreover, during the test, the lubricator stand was constantly vibrated by a small eccentric electric motor to promote the separation and/or stratification of the oils.

The results confirmed those from the centrifuge test of Example 3. The oil of Example 1 showed no tendency to separate or stratify under these conditions. In addition,

the critical system components, including the filter and Example The Example 1 oil also had other required textilemachine oil properties. The Example 1 oil was subjected to a special test to measure the retention or anti-leak charatcteristics of machine oils. The test correlates with the field performance, and for this reason was used to compare the Example 1 oil with the Example 2 oil and with a conventional machine oil which contained no additives to improve oil retention.

The special test apparatus was a combination of iron nipples, union sleeves, and elbows. They were joined together hand tight in a U-shape and spot-welded to hold a fixed position. In the test 300 ml. of oil were poured into the apparatus and it was then pressurized to 30 p.s.i. with nitrogen and allowed to stand at the selected test temperature for one hour. The oil that leaked from the apparatus was collected and weighed.

There was no significant difference in leakage between the Example 1 and Example 2 oil, both giving about times less leakage than the conventional oil.

However, the Example 1 oil has a leak-reducing feature not found in the Example 2 oil. The Example 1 oil keeps rubber seals soft and pliable and causes them to swell slightly, thus, eliminating afield usage problem of seal shrinkage. The difference between the Example 1 and Example 2 oils is demonstrated by the following lab 'data:

Rubber Swell Test, percent, 212 -F., 168 hrs.

Example 1 oil +8.2 Example 2 oil -0.1

Buna N seals swell in the Example 1 oil and, thus, keep snug tolerances and prevent leakage which takes place in usage due to wear.

Thus, the Example 1 lubricant has a combination of good retention properties plus the seal-conditioning feature which results in less stray oil in textile plants than with the Example 2 lubricant.

Example 6 Even with the excellent retention properties of the Example 1 lubricant, in field usage it will occasionally come into contact with cloth. It is important, therefore, that the oil not weaken the fabric after the finishing steps are completed.

The damaging potential of textile machine oils can be evaluated by the method of the Institute of Textile Technogoly (I'IT). In the evaluation, the test oil is run for eight hours in a laboratory-mounted bearing to simulate used lubricant conditions. During this period, the bearing temperature is recorded (it was essentially the same for the lubricant of Example 1 and the lubricant of Example 2, running between 105 and 110 F.).

When the sample preparation is' complete;'the'oil is" applied to desized cotton test fabric. Before bleaching,

one-half of the contaminated fabric samples, as well ascontrol pieces, are treated with 1% sulfuric acid solution for 30 minutes. The test pieces are then boiled one hour in 2% caustic, rinsed with tap water, bleached with a hydrogen peroxide solution for one hour, rinsed and dried. The samples and controls are then subjected to a "armpit -LLllQILQQI. 2

Fabric break strength, percentof control sample:

With acid treatment, 97. 6 94. 8 Without acid treatment 87.8 89. 1

These data show that both are excellent in terms of cloth scourability with minimum fiber damage.

The Example 1 oil also produced less staining of cloth. These test results caused the Example 1 oil to obtain the highest possible I'IT rating and make it applicable in all textile plants.

Example 7 Commercial lubricants Example 1 Description B C D lubricant l Loom test:

Gear temperature, F.

Motor side +17 +44 +30 +17 Other side +45 +36 +17 Power costs, percen +5. 5 +7. 9 5. 7 Overall performance. Unsatisfactory Satisfactory Average of two tests. 3 Data relative to Example 2 oil.

The Example 1 lubricant was the only oil which provided power savings. The temperature differences were not considered significant. Oil B was Gulf Harmony 121, Oil C was Texaco Rock Drill 1543' and Oil D was Humble Nuto 113.

In a test at another southern mill, the lubricating properties of the Example 1 lube were found to equal those of the Example 2 oil, but the Example 1 oil had better staining and removal properties. No separation problems were note The examples above show that the Example 1 lubricant not only solves the separation problem noted occasionally in the field with prior art oils, but it also has lighter color and brighter appearance and causes less staining should it come in contact with fabric during manufacture.

In addition to the stability. and appearance, the Example 1 lubricant conditions and protects rubber seals and provides lower mill power consumption and cost. The Example 1 oil is also useful as a military automotive and artillery grease. The preferred range (ISO- F.) of aniline point. for the base oil disclosed herein is not necessarily the preferred range if non-hydrocarbon seal swelling agents are contained in the lubricant. For other rubbers than buna-N, neoprene, -etc., such asthe silicones a diiferent aniline point range may be required for proper swellin (e.g.,- -for silicone rubbers an; aniline point in the a range 0f-195-2 15. F. is preferred).

'Thefollowing" Table lflists the properties of the textile'-" machinery lubricant of Example l, which is a lubricant of the present invention. The table also lists a preferred range for these properties; however, the lubricant of the present invention'need not have properties within thisrange.

Tables 2 and 3list typical properties of commercially available naphthenic'lubes (before and after hydrorefining) which can be used in practice of the present invention. The distillate oils are sold under the trade name Circosol and the hydrorefinedoils are sold under the trade name Sunthene.

TABLE 1 Preferred range Property Method 1 Example 1 of properties Viscosity, MacMichaei/70" F--. 25 20-35. Flue ,CO F D92 280 270min. Fire, COG, F- D 330. 310 min.

our, F D97 20 Color D1600 2.5. 3.5 max. AP arnnm Visual Slight haze p Copper strip, class, 212 F., 3 hr Sulfur, percent- Conradson carbon, percent- Aniline point, F

Ash, nnronnt Suliated ash- Foam, tendencyfstability Sequence 1, ml- Sequence 11, ml Sequence 111, ml.

Busting, distilled wa 50/0 max. 50/0 max. Pass.

4-ball wear scar: 25 kg., 1,800 Lithium, p D m Chlorine, percent l ASTM test method numbers.

1 Calculated from data obtained by picnometer. Accurate results cannot be obtained using a hydrometer.

TABLE 2.TYPICAL DATA, COMMERCIALLY AVAILABLE HYDROREFINED NAPHTHENIC LUBES Property ASTM test 011 1 Oil 2 Oil 3 Oil 4 Oil 5 Oil 6 Oil 7 Oil 8 Viscosity, SUS at 100 F D2l6166 104 155 210 502 780 1, 275 2, 206 5,0 Viscosity, SUS at 210 F D2l6166 38. 41. 0 43. 1 52. 0 59. 0 67. 7 84. 7 126. API Gravity at 60 F 13-287-67 24. 2 23. 3 22. 5 20. 6 19. 9 19. 3 18. 6 19. 0 S 1110 gravity at 60 F D-1250-56 9088 9140 9190 9303 9350 9380 9427 9402 ash point, 000, F D-92 66 330 335 345 385 365 400 440 470 Volatility, 22 hours at 225 F. wt. percent D 972-56 6. 38 5. 4. 57 2. 53 1.81 1. 00 0.23 0. 02 Pour point F D-97-06 30 -25 -1O -5 0 +15 +20 color, 151 11 13-1500 13-15110-64 0.5 0.5 0.5 1.0 1.0 1.0 1.5 1.5 U.V. absorptivity at 260 mu D-2008-68 2. 2 3. 0 3. 4 4. 1 4. 8 5. 3 5. 7 6.7 M hammwnivht '.D250267 205 325 330 355 370 380 400 450 Viscosity-gravity constant D-2501-67 .871 .873 .875 878 .881 .881 .882 .871 Refractive index, n D-1747-62 1.4986 1.5015 1.5039 1.5104 1. 5130 1. 5146 1. 5170 1. 5174 Reflectivity intercept D-2159-64 1.0460 1. 0463 1. 0463 1. 0471 1. 0473 1. 0474 1. 0475 1. 0491 Carbon type analysis:

Aromatic carbon atoms, C... percent 15 16 16 15 17 18 18 1s Naphthenic carbon atoms, (30, Percent D-2i40-62 42 42 42 43 41 41 41 36 Paraflmic carbon atoms, Cg, percent 43 42 42 42 41 41 41 46 Molecular type analysis (clay gel):

Asphaltenes, wt. percent 0 0 0 0 0 0 0 0 Polar compounds, Wt. percent 0. 2 0. 4 0. 5 0. 7 0.8 1.0 1. 1 2. 0

Aromatics, wt. percent..- D-2007- 34. 8 37. 6 38.5 42. 3 43. 2 43. 0 43. 9 41. 8

Total aromatics, wt. per 35. 0 38. 0 39. 0 43.0 44. 0 44.0 46. 0 43. 8

saturates, wt. percent 65. 0 62. 0 61. 0 57. 0 56.0 56. 0 55. 0 56. 2 Aniline point, F D611-64 156 160 162 164 171 174. 0 176. 0 193 ASTM type D-2226-69 103 103 103 103 103 103 103 103 Norm-Oils 2, 3, 5 and B are blends oi oils 1 and 7.

TABLE 3.-TYPICAL DATA, COMMERCIALLY AVAILABLE NAPHTHENIC DISTILLATE OILS ASTM ASTM Property designation 011 A Oil N o. 3 011 B 011 0 011 D Oil E 011 F 011 G 011 H Viscosity, sus at F D-2161-c6 108 156 208 310 515 730 1,276 2, 525 5,945 Viscosity, SUS at 210 F- Ill-2161 60 38. 2 41 43.2 46. 8 52. 4 58. 8 68 87. 2 135 API gravityo! 60 F"--- D-287-67 22. 2 22. 4 21. 0 20. 1 19. 6 19. 1 18. 4 17. 6 17. 3 Specific gravity at 60 F D-1250-56 9206 9194 .9279 9334 9365 9396 9440 9490 9509 F ash 101111, 000, F D-92-66 e20 330 345 355 380 330 495 Volati ty 22 hrs. at 225 F., wt. percent"--- D-972-50 7. 58 5. 96 5. 40 4.35 3. 08 2. 11 l. 67 0.16 0.02 Pour point F 9766 -15 35 -30 -15 -10 -5 0 +10 +20 0010 101 11 13-1500 134500-34 1. 25 1. 75 1.15 2.0 2.0 2.5 3.0 3.5 5. 75 M l ular w ight D-2502-67 295 325 325 345 355 370 380 395 450 Viscosity-gravity constant D- 501-6 0.884 0.878 0.884 0.887 0.885 0. 885 0. 885 0.889 0. 884 Relractive index D-1747-62 1- 5031 l- 5079 1. 5121 1. 5160 1. 5167 1. 5190 1. 5210 1. 5222 1. 5250 Beiractivity intercept 13-2159-64 1. 0502 1. 0479 1. 0500 1. 0511 1. 0503 1. 0510 1. 0508 1. 0495 1. 0495 Carbon type analysis:

Aromatic carbon atoms, 0. percent 21 20 21 22 21 22 22 21 2o Naphthenic carbon atoms, C percent- D-2140-62 37 36 37 36 37 30 36 39 38 Paraflnic carbon atoms, 0.. percent 42 44 42 42 42 42 46 4o 42 Molecular type analysis (clay gel):

As haltenes, wt. percent-....'. 0 0 0 O 0 0 0 0 0 Po Compounds, wt. percent. 1. 1 1. 2 1. 8 2.0 2. 5 2. 7 8. 0 2. 7 4. 2

Aromatics, wt. percent.. D-2007-56'l 43. 0 41. 7 44. 0 44. 0 43. 8 43. 6 44. 0 44. 8 44. 7

Total aromatics, percent 44. 1 42. 9 45. 8 46. 0 46. 3 46. 3 47. 0 47. 5 48. 9

saturates, wt. percent 55.9 57. 1 54. 2 54. 0 53. 7 53.7 53. 0 52. 5 51. 1 Aniline point, F D-611-04 156 152 154 156 162 166 172 183 ASTM type 13-2226-09 103 103 103 103 103 103 103 103 103 Norm-Oils B, C, E and F are blends 0! oils A and G.

' the range of 40-12,000 SUS at 100 F said tackiness agent polymer, and natural rubber obtained from dehydrated.

0.01-0.4 and an aniline point in the range of ISO- F.,

and containing in the range of 85-100% of at least one hybeing selected from the group consisting of polyacrylates, aluminum oleate, olefin polymer, hydrogenated olefin polymer, mixtures of hydrogenated and unhydrogenated olefin latex.

2. A lubricant according to claim 1 wherein said base oil contains a wide boiling range blend of at least two bydrorefined naphthenic oil component having a viscosity in 75 drorefined naphthenic oils.

3. A lubricant according to claim 1 and having a Mac- Michael viscosity in the range of 20-35 and wherein said base oil has a viscosity at 100 F. in the range of 125- 300 SUS.

4. A lubricant according to claim 3 wherein said tackiness agent is polyisobutylene or hydrogenated polyisobutylene or a mixture of polyisobutylene and hydrogenated polyisobutylene.

5. A lubricant according to claim 4 and containing 0.1- 1.5% lithium stearate.

6. A lubricant according to claim 5 and containing 03-10% of a chlorinated parafiin or 0.22% of tricresyl phosphate, as an antiwear agent.

7. A lubricant according to claim 6 and containing 0.5- 20 p.p.m. of a silicone antifoam.

8. A lubricant according to claim 7 and containing 0.05-1% of ditertiarybutyl paracresol as an antioxidant.

9. A lubricant according to claim 1 wherein said base oil contains in the range of 05-15% of hydrorefined paraffinic oil, solvent-refined parafiinic oil, naphthenic distil- 20 late or naphthenic-acid free naphthenic distillate.

10. A lubricant according to claim 1 where the aniline point of said hydrorefined naphthenic oil component is in the range of ISO-170 F.

11. Hydraulic oil according to claim 1 wherein said lithium soap is a soap of a C -C fatty acid.

ness agent is selected from the group consisting of polyacrylates, hydrogenated olefin polymer, mixtures of hydrogenated and unhydrogenated olefin polymer and natural rubber obtained from dehydrated latex.

References Cited UNITED STATES PATENTS Mikeska et a1. 25249.8 X Prutton 252-42.1 X Morgan 252-36 Bax et al 252---36 Coshburn 25236 X Griifith et a1 2524'1 X PATRICK P. GARVIN, Primary Examiner A. H. METZ, Assistant Examiner U.S. Cl. X.R.