US3663281A

US3663281A - An asphaltic composition

Info

Publication number: US3663281A
Application number: US86974A
Authority: US
Inventors: Eugene M Fauber
Original assignee: EUGENE M FAUBER
Current assignee: EUGENE M FAUBER
Priority date: 1970-11-04
Filing date: 1970-11-04
Publication date: 1972-05-16
Anticipated expiration: 1989-05-16

Abstract

Asphaltic compositions are prepared having suitable softening points, needle penetration and stain values for use in paper laminates. These compositions are prepared by airblowing a blend of a major amount of asphalt and a minor amount of foots oil derived from slack wax from a medium lubricating oil distillate.

Description

United States Patent Fauber 51 May 16, 1972 [54] ASPHALTIC COMPOSITION [72] Inventor: Eugene M. Fauber, 6941 Stateline Avenue, Hammond, Ind. 46324 [22] Filed: Nov. 4, 1970 I21] Appl, No; 86,974

Related US. Application Data [63] Continuation-impart of Ser. No. 727,075, May 6,

1968, abandoned.

[52] US. Cl ..l06/279, 208/18, 208/22, 208/39 [51] Int. Cl ..C08h 13/00, C08h 17/22, C08i 1/46 [58] Field of Search ..106/273-285, 270-271, 106/311; 208/3, 4, 6,11,18, 23, 44, 39, 21, 40

[56] References Cited UNITED STATES PATENTS 2,069,927 2/1937 Rhodes et a1. 106/278 X Primary Examiner.loan B. Evans Attorney-Thomas J Clough and Robert J. Mawhinney [5 7] ABSTRACT Asphaltic compositions are prepared having suitable softening points, needle penetration and stain values for use in paper laminates. These compositions are prepared by airblowing a blend of a major amount of asphalt and a minor amount of foots oil derived from slack wax from a medium lubricating oil distillate.

8 Claims, No Drawings ASPHALTIC COMPOSITION This application is a continuation-in-part of application Ser. No. 727,075, now abandoned.

This invention relates to novel asphaltic compositions comprising asphalt-foots oil combinations suitable, for example, for use as paper laminates. More specifically, this invention relates to blends of asphalt and foots oil which are suitable for use in making paper laminates and which are produced by airblowing a blend of asphalt and a foots oil fraction from the production of paraffin wax.

in order to be useful for making paper laminates it is necessary that asphalts employed have acceptable softening point (e.g. about l852l5 F., R&B), needle penetration (e.g. about 20-50 at 77 F.) and stain test values (e.g. Barber Stain Value in the range from 1 to 2, preferably 1). If the asphalt has too low a softening point, it has a tendency to flow at elevated temperatures thus permitting lateral movement of the laminated paper sheets with respect to one another. If the needle penetration is too low, the laminate lacks flexibility. High stain values (e.g. Barber Stain Value greater than 2) result in an unsightly product. Inasmuch as the asphaltic residues from crude oil may not possess acceptable properties, some sort of treatment is often required before the asphalt can be used to make laminates. It is known that the properties of asphaltic residues may be altered by air oxidation, specifically by airblowing. However, many of these asphaltic residues, when airblown to a satisfactory softening point to be used in preparing laminates,'are then found to have too low a penetration or too high a stain value to be satisfactory.

It is well known that if an asphaltic material airblows to give too low a penetration for a desired softening point, petroleum gas oils of various types can be added to the asphalt before airblowing to cause higher, and in some cases much higher, penetration for a given softening point than would have been obtained by airblowing the asphalt alone. However, petroleum gas oil, while permitting a higher penetration when the asphalt is air blown to the desired softening point, also cause undesirably high stain test values (e. g., Barber Stain Values greater than 2).

It is, therefore, an object of the present invention to prepare an asphaltic composition suitable for use in preparing paper laminates. More specifically, it is an object of this invention to provide an asphalt composition which can be airblown to give a product having satisfactory needle penetration, softening point and stain test values to be used in the preparation of laminates constructed, for example, from kraft paper or corrugated paper or board.

These and other objects of the present invention are accomplished by an asphaltic composition which comprises an airblown mixture of a major amount (i.e. greater than 50 percent by weight) of asphalt and a minor amount, often about 0.5 percent to about 20 percent by weight, preferably about 2.5 percent to about percent by weight based on the total asphaltic composition, of a first pass foots oil fraction obtained from medium slack wax. The composition is airblown to the desired softening point. It has been found that the resulting airblown product, unlike unmodified asphalts, also gives satisfactory penetration and stain test values.

The foots oil of this invention is a by-product in the production of paraffin wax and is the first foots oil fraction obtained from slack wax derived from a medium lubricating oil distilled from a mineral oil. The foots oil can be prepared in the following manner. A waxy petroleum crude oil is fed to a crude still and various cuts are taken off including a cut called medium lube distillate which is the primary source of the foots oil used in this invention and which boils primarily in the range of about 700-l ,000 F., preferably about 800-900 F and has an A.P.l. specific gravity of about 26, e.g. about 25.5 to 26.5. This medium lube distillate may advantageously be further refined to improve color stability by solvent extraction using, for example, phenol or furfural to remove aromatic type compounds. The lube distillate or the raffinate from solvent extraction is further refined by dewaxing, often at relatively low temperatures of, for example, about -l0 F using various solvents or mixtures of solvents such as methyl ethyl ketone, benzene, acetone, and toluene to produce, after removal of the solvent, what is called a base lube oil stock and a slack wax. The slack wax is further refined to produce a deoiled slack wax and a foots oil, for instance, by further solvent extraction, using the same solvents but at higher temperatures, e.g. about 45 F as in the dewaxing step above or by sweating.

The foots oil of this invention is relatively low in aromatic compounds and is composed principally of n-paraffins, isoparafilns and monocyclic naphthenes. More specifically, the composition of the foots oil of this invention is typically, by weight, about 40-50 percent n-paraffins, about 5-15 percent iso-paraffins, about 35-45 percent monocyclic naphthenes and about 1-5 percent aromatics. The properties and composition of a typical foots oil composition, made by the process described, are shown in Tables I and II respectively.

TABLE I Properties of lst foots oil from medium slack wax TABLE II Composition by Mass Spectrometer Analysis Carbon no. distribution iso-Paraffins monocyclic- Naphthenes aromatics Asphalts which may be altered by the addition of the foots oil of this invention to have suitable airblowing characteristics to be used as laminating asphalts are asphaltic residues from mineral crude oils. These asphalts have a needle penetration (ASTM-DS) at 77 F. in the range of about to 300, and often have softening points of about 95-l 10 F.

Air-blowing of the foots oil-asphalt composition of this invention can be carried out at temperatures of about 400 to 600 F often about 450 to 550 F. for a period of time sufficient to give a softening point of about to 220 F., preferably about 208-2l2 F., and a needle penetration of about 20 to 50, preferably about 20-25 at 77 F. For example, airblowing can be carried out at a temperature of 500 F. with 3.3 cu. ft. of air per hour per lb. of foots oil-asphalt charge. Airblown foots oil-asphalt composition of this invention can be produced to meet laminating asphalt specifications of at least about 20, e.g. -25 penetration at 77 F., 208-212 F. softening point (R&B), and Barber Stain Value in the: range of 1 to 2, preferably 1. Compositions prepared by the process of this invention were tested using ASTM-D36, Standard Method of Test for Softening Point of Bituminous Materials, Ring and Ball Method, and ASTM-DS, Standard Method of Test for Penetration of Bituminous Materials.

Stain values were obtained using the Barber Stain Test. in the Barber Stain Test i gram of the bituminous material is weighed to the nearest 0.05 gram and placed between two pads of cigarette papers, each containing 12 3 X 4 inch sheets. The papers are placed in an over at 130 F. for 120 hours under a 3 oz. tin filled with shot weighing 400 grams. The stain value is the number of stained sheets below and above the sample divided by two, counting the sheet next to the sample as one. The cigarette paper used in the comparative tests was No. 4 Washington grade.

Compositions were formulated as shown in Table lll.

The asphalt employed in the compositions shown in Table lll was made from mixed Mid Continent and Wyoming crudes by steam and vacuum distillation and tested as follows:

Penetration at 77F. 205 Softening Point (R&B), F. 102 Flash, COC, F. 620

Fire, COC, F. 710 Viscosity, SSF at 275F. 93 lnsolubles in CCl. Wt.% 0.23 Oliensis Spot Test Negative Specific Gravity at 60F. 1.0002

The gas oil employed in the compositions shown in Table lll was made by distillation of crude petroleum oil and tested as follows:

Gravity, APl 23.7 Flash, COC, F. 485 Fire, COC, F. 545 Viscosity, Kinematic at 210F. 12.54

The gas oil was composed primarily of saturated (paraffins and naphthenes). This gas oil was analyzed by means of the standard clay-gel absorption chromatographic method (ASTM D 2007-69) and was shown to have the following composition:

Weight Saturates 54.2 Petroleum Resins 14.1 Aromatics 31.7

The foots oil employed in these compositions was prepared as previously described and had the properties and composition shown in Tables I and II.

Following their formulation, the compositions shown in Table lll were airblown to produce the asphalt compositions shown in Table IV.

TABLE IV Air Blown Composition A B C D Penetration 1 3 i6 20 20 Softening Point (R&B),F. 210 210 210 210 Barber Stain Value 1 3 4 1 It may be seen that the asphalt alone (composition A) when airblown to a softening point suitable for laminating (210 F.) has an acceptable Barber Stain Test value but is much too low in penetration to be acceptable. The addition of 7 percent by weight of gas oil to the asphalt (composition B) resulted in a product acceptable in softening point but having too high a stain test value and too low in penetration. The addition of 15 percent by weight of gas oil to the asphalt (composition C) resulted in a product acceptable in penetration and softening point but having too high a stain test value. Addition of only 7 percent by weight of the foots oil of this invention to the asphalt (composition D), however, yielded an asphalt having completely satisfactory softening point, penetration and stain test values for laminating. These results are particularly surprising in view of the fact that both the gas oil and foots oil are composed primarily of saturated compounds (i.e., paraffins and naphthenes).

While this invention has been described with respect to various specific examples and embodiments, it is to be understood that the invention is not limited thereto and that it can be variously practiced within the scope of the following claims.

The embodiments of the invention in which an exclusive property or privilege is claimed are defined as follows:

1. An asphaltic composition which comprises an airblown mixture of at least 50 percent by weight of an asphalt having a needle penetration at 77 F. of about 150 to about 300 and a softening point (R B) of about F. to about 1 10 F. and between about 0.5 percent and about 20 percent by weight based on said asphaltic composition of a first pass foots oil from slack wax obtained from a waxy medium lube mineral oil distillate boiling primarily in the range of about 700 to l,000 F said foots oil comprising about 40 50 weight percent nparaffins, about 5 to 15 weight percent iso-paraffins, about 35 to 45 weight percent monocyclic naphthenes and about 1 to 5 weight percent aromatics, and said asphaltic composition having a softening point (R B) ofabout 185 F. to about 220 F., a needle penetration of about 20 to S0 at 77 F. and a Barber Stain Value in the range of from i to 2.

2. The composition of claim 1, which contains about 2.5 to about 10 percent by weight of said foots oil.

3. The composition of claim 1, wherein said asphaltic composition has a softening point of about 208"-2l2 F., and a needle penetration of about 20-25.

4. The composition of claim 1, wherein said first pass foots oil has a softening point of about F.

5. The composition of claim 4, wherein said first pass foots oil has a softening point of about 100 F.

6. The composition of claim 1, wherein said composition has a Barber Stain Value of l.

7. The composition of claim 3, wherein said composition has a Barber Stain Value of l.

8. The composition of claim 5, wherein said composition has a Barber Stain Value of l.

I l i I i

Claims

2. The composition of claim 1, which contains about 2.5 to about 10 percent by weight of said foots oil.
3. The composition of claim 1, wherein said asphaltic composition has a softening point of about 208*-212* F., and a needle penetration of about 20-25.
4. The composition of claim 1, wherein said first pass foots oil has a softening point of about 100* F.
5. The composition of claim 4, wherein said first pass foots oil has a softening point of about 100* F.
6. The composition of claim 1, wherein said composition has a Barber Stain Value of 1.
7. The composition of claim 3, wherein said composition has a Barber Stain Value of 1.
8. The composition of claim 5, wherein said composition has a Barber Stain Value of 1.