US2457848A - Floor and wall covering - Google Patents

Description

Jan. 4, 1949. w. STUBBLEBINE FLOOR AND WALL CVOVERING 2 Shawna-sheenl 1 Filed July 31, 1943 FIG.

Jan. 4, 1949.

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PERCENT INITIAL gnam/who@ Patented Jan. 4, 1949 2,457,848 l C E FLOOR ANI) WALL COVERING Warren Stubblebine, Manheim Township, Lancaster County, Pa., assignor to Armstrong Cork Company, Lancaster, Pa., a corporation of Pennsylvania Application July 31, 1943, Serial N0. 496,967

9 Claims.

This invention relates to licor and wall coverings and more particularly to a floor or wall covering suitable for use in structures where free alkali is present and capable of withstanding adverse conditions which would normally completely deteriorate linoleum type coverings.

In modern homes, it is common practice to utilize a portion of the basement for recreation rooms, bars, and the like, and, in order that the floors and walls may have an attractive appearance, they are either painted or covered with a flexible hard surface covering. Where the iioor and wall surfaces are below grade, there is the problem of. providing a covering which is not deleteriously attacked by the free alkali which appears at the surface of the concrete .iloor and wall areas, aggravated by water which is generally always present in below grade installations. All oil paints are unsatisfactory for this purpose and special alkali resistant paints have been devel- 90 oped for this use. Linoleum floor and wall coverings, while ideally suited from the standpoint of decoration, are so badly affected by alkali that they cannot be used. Asphalt tile is suitable for this purpose because the asphalt binder is not saponiled by the free alkali. Tiles made with an asphalt binder, however, are not attractive because of their dark colors and, as a consequence, especially developed binders have been produced which are resistant to such attack. These tiles are generally installed in pieces, say 9" x 9" squares, and when unusual effects are desired, the tile mustbe heated and cut and this can be accomplished only with great skill and at considerable expense. Tiles of this sort are no1; generally used on wall surfaces because of their cost and also becausethey are designed primarily for withstanding wear and are consequently relatively thick. Even with these special binders, the colors available are relatively limited, being generally in the darker shades.

There is also a demand for a flexible hard surface floor covering which can be applied directly to concrete, such as suspended concrete floors, which has just set, without waiting'the usual period of three months for iinal curing of the concrete. In this condition, there is considerable free alkali present until nal curing has been accomplished and the ilexible floor coverings now available; such as linoleum, cannot' be installed immediately after the cement has hardened, but

installation must be delayed until months after Vthe building has been completed.

It is an object of my invention to provide a exible hard surface floor or wall covering which is capable of withstanding attack by i'ree alkali without materially changing its physical characteristics, such as initial penetration, residual indentation, flexibility, resilience, surface hardness, or wear resistance, and which-may be safely incorporated into a building structure in which 2 there is a base such as a concrete iloor or wall surface, where free alkali is present or made available through a leaching effect, particularly induced by water present in below grade installations.

Another object of my invention is to provide a flexible hard surface floor or wallcovering which may be incorporated into such structures and which may be produced in substantially continuous lengths without necessity for curing or stoving as is common practice in the manufacture of linoleum.

In attaining these objects, I provide a. covering which is suitable for general iioor and wall covering uses, having unusual characteristics; particularly good exibility, low initial penetration and residual indentation, and high resistance to alkali, such as present in strong soaps and cleaning powders.

Floor or wall coverings, in order to be acceptable, should meet the minimum specications set out in Federal speciilcation LLL-L-367, dated September 15, 1942, with respect to indentation under item E-4 and pliability under item E-6. In the-indentation test, a disc of the covering material is supported upon a steel plate and a pressure of 3,200 pounds per square inch is applied to the upper surface of the sample for a period of thirty seconds by means of a fiat-ended cylindrical steel bar 0.178 inch in diameter. The load is lowered gently until the bar is in full contact with the sample and the sample in full contact with the plate. 'After thirty seconds, the load is quickly and completely removed. Sixty minutes after removal of the load the residual indentation is measured to the nearest thousandth of an inch and calculated as percentage of the original thickness. This percentage gure is known as the per cent of residual indentation and, in accordance with the Federal specification referred to, must not exceed 10%. The penetration of the bar into the sample at the end of the thirty seconds application of pressure is also measured and this is known as the initial penetration. While the Federal specifications have no specic provision for initial penetration, the oor covering industry generally considers a product unsatisfactory if the initial penetration is greater than 50%. vvWhere the terms initial penetration" and "residua1`indentation are used herein, I mean the initial penetration and residual indentation determined in accordance with the foregoing procedure.

The pliability test is determined by cutting a strip 2 inches wide by 8 inches long longitudinally of the covering and a similar strip of the same size transversely of the covering. These strips are bent with the backing, if one is employed, on the inside. The bend is made at approximately the` center of 'the sample over a mandrel 2V: inches in diameter to an arc of 180 and at dium hydroxide, and linseed oil tests.

approximatelyV a uniform speed in approximately 5 seconds. Any breaking or cracking is noted and, if so little as surface cracks appear, the product is unacceptable.

A test which is believed to be more indicative of the exibility of oor covering products and one which has been employed by the linoleum industry is the so-called Tinius-Olsen Stillness test. This test is also commonly used in the testing of wire, tinplate, felt, and other materials. One-eighth inch linoleum, when tested by this method on a Tinius-Olsen machine, shows a break angle of about 50 and a per cent of weight of about 60% to 65%. These results do not materially change over long periods of time, indicating that linoleum is a relatively stable product with respect to exibility. The trade expects any product which will be used for floor and wall covering purposes to possess at least an equivalent degree of iiexibility.

Other tests commonly employed to determine the physical characteristics of hard surface floor coverings are water immersion, soap solution, so-

of these tests,the sample is immersed in the treating solution for 18 hours at a temperature of '70 F. The samples are removed from the solution, wiped dry, and thengiven the standard initial penetration and residual indentation test above described in connection with Federal specification IIL-1F36?. In the soap test, a neutral 1% soap In each solution is used and this test gives a general indication of the effect on indentation resulting from frequent washing with mild soaps. The

sodium hydroxide test in which the sample is immersed in a 2% sodium hydroxide solution is of particular importance, for by this test it is possible to determine whether a floor covering is satisfactory for use in those structures where it will be brought into contact with free alkali. It has been determined that those materials which havel an initial pentration greater than '15% in this test are wholly unsuited for this purpose. As a matter of fact, those materials which show an initial penetration greater than are not desirable. Products like linoleum are completely dissolved in a 2% sodium hydroxide solution in about 6 hours, indicating clearly that such products are not satisfactory for this use. This test also shows the durability of the product under unsatisfactory cleaning conditions where harsh soaps and cleaners are used.

'I'he covering of this invention is formed with a binder composed of a special phenol-modified coumarone-indene resin modified with a cellulose ether such as ethylcellulose. The phenol-modiiied coumarone-indene resin employed may be produced by the simultaneous polymerization and reaction of the polymerizables contained in hydrocarbon liquids such as crude solvent naphtha and a phenol or phenolic substance. More specifically, the resin can be prepared by mixing and heating crude solvent naphtha and cresol with activated clay at a temperature of about C. to C. until a resin is formed. The reacted mixture is filtered to remove the activated clay and the mixture is then subjected to an initial distillation to remove the nonpolymerizable portion of the naphtha and any unreacted cresol. The residue is separated by steam distillation into a relatively hard resin fraction and a heavy viscous resin fraction having a melting point between 5 C. and 15 C. as determined by the cube in mercury test. It is this heavy viscous fraction 4 suitable since it does not have the desirable effect of toughening and improving the working characteristics of the composition. The phenol-modied coumarone-indene resin so prepared possesses some unusual characteristics which make it ideally suited for my purpose. While I do not wish to be limited to any theory. it is my belief that there is a particular -OH grouping in the resin which results in the unusual properties which are obtained when this material is combined with a cellulose ether in the preparation of my binder. One distinguishing chemical characteristic of this resin is that it is soluble in alcohol, whereas other resins of a similar nature having higher melting points are not soluble in such solvent. By the term alcohol soluble phenolmodiied coumarone-indene resin having a melting point between 5 C. and 15 C., as recited hereinafter in the specification and claims, I mean a product such as that obtained in accordance with the procedure set forth above, or one that is substantially identical with it even though prepared by a different procedure.

While I prefer to use ethylcellulose as a modiiier in combination with the phenol-modified coumarone-indene resin, other cellulose ethers such as benzylcellulose or any other cellulose ether which is compatible with the phenol-modifled coumarone-indene resin may be employed. The phenol-modified coumarone-indene resin constitutes the major portion of the binder and preferably is in the order of about 55% to 65% of the total binder. A specific example of the binder is as follows. Parts by weight Alcohol soluble phenol-modified coumaroneindene resin having a melting point between 5 C. and 15 C 125 Ethylcellulose '25 This binder has a melting point between 103 C. and 112 C. and is prepared by charging the resin into a mixing kettle heated to about 300 F. The ethylcellulose is then charged into the kettle containing the resin and agitation is accomplished to effect an intimate distribution. Upon heating, the materials are dissolved and are combined to form a highly viscous binder. This viscous mass is then charged into a mixer, such as a Werner- Pfleiderer mixer, and the llers and-pigments are there added. The mixer is heated to about 300 F.

A typical oor or wall covering composition is asfollows. by weight Binder prepared as above Serpentine l 225 Ground limestone 210 Cork dust 50. Coloring pigments 45 longer mixing time than those of a coarser nature. After a homogeneous mixture has been obtained, the batch is discharged from the german mixer into a two-roll scratcher, which is effective for breaking the mass into fine particles suitable for calendering. The .granules are then calenwhich I employ. The hard resin portion is un- 15 dered. At this point in the operation, a backing.

such as burlap or cotton fabric or asphalt saturated felt, or the like may be used. I wish it to be understood that the covering of this invention possesses suilicieiit strength that a backing is not required. The calender is generally of the tworoll type having a heated face roll and a cooled back roll. The face roll may be heated from 250 F. to 300 F. so as to produce a finished sheet having a high gloss exposed surface, and the back roll is preferably maintained at 100 F. or less.

The material as it comes from the calender roll is completely finished and ready for use upon cooling. This should be contrasted to the usual type linoleum floor coverings where, after calendering, the material must be hung in heated curing stoves for periods ranging from 6 days to 3 weeks. Where the quantity produced by a man-- ufacturer is relatively large, the stove capacity is a major factor in limiting production.y With the covering of my invention, all of this equipment is` dispensed with and the product as calendered is run through a cooling zone and then and packaged for shipment.

From the foregoing specific example, it will be observed that the binder comprises about 25% of the total weight of the mass. Preferably, the binder is in the order of to 40% and the liller is from about 60% to 80%. The particular type of fillers chosen is not important. Satisfactory results have been obtained where both organic and inorganic fillers have been used. My composition is of a resiient nature even with mineral fillers and, accordingly, it is not necessary to use a high percentage of resilient organic type lling materials, such as cork or wood flour commonly used in the manufacture of linoleum to impart the desired resilience. Organic fillers are general'y much more expensive than inorganic llers and many are subject to attack by alkali. With my composition, the ratio of llers to binder may be extremely high and good ilexibility and resilience will obtain, thus decreasrolled up ing the cost of the product and making the use of large quantities of organic fillers which may be bady attacked unnecessary. This is due to the unusually good binding value of the binder of my composition. In myresearch work on this problem, I tried various compositions in which cellulose ether was modified and others in which cellulose ether was the modifier and, in practically all instances. it was impossible to incorporate as much as 50% of filler; most compositions satisfactorily held only to 40% of filler.

I have found that where both organic and inorganic flllers are employed a ratio of organic to inorganic llers of from 1 to 6 and from 1 to 9 is desirable, and satisfactory results have been obtained when one part by Weight of organic filler, such as cork, is used with 8 parts of inorganic liiler such as serpentine and ground limestone,

as in the specific example given above.

An example of a binder utilizing another cellulose ether is as follows:

Parts by weight yAlcohol soluble phenol-modified coumaroneindene resin 100 Benzylcellulose 52 Reference is made to the attached drawings, in which Figure 1 is a diagrammatic view showing my covering applied to a concrete base such as a floor;

Figure 2 is a similar view showing a modified covering applied to a plastered wall surface;

Figure 3 is a chart which illustrates the physical properties of my material;

Figure 4 is a table comparing the Tinius-Olsen Stiifness test on my composition with that of linoleum; and

Figure 5 ls a graph illustrating the effect on initial penetration resulting from aging.

Referring to Figure 1, there is shown 'a base 2 which may be a fresh laid concrete floor or floor below grade to which ordinary linoleum type hard surface iloor or wall coverings could not be satisfactorily applied. Adhesively secured to the base 2 by a layer of adhesive 3 is a covering 4 composed of a backing layer 5 and a wearing layer 6. The wearing layer 6 is of the composition referred to above, formed of filler and pigment particles and a binder composed of alcohol soluble phenol-modified coumarone-indene having a melting point of 5 C. to 15 C. and a cellulose ether.

Figure 2 shows a modification of my invention in which the base 2 is a plastered. wall surface which has a covering 4 adhesively secured there- 'to by a layer 3', the covering having no backing or foundation layer such as the layer 5 of Figure 1.

Reference is now made to the chart constituting Figure 3. From this it will be observed that the product of this invention is not substantially affected by water, a 1% soap solution, or linseed oil. The really significant factor, however, is the result obtained on the 2% sodium hydroxide test. Referring specifically to this portion of Figure 3, it will be noted that the control specimen shows an initial penetration of about 29%. The sample treated with the 2 sodium hydroxide shows substantially identical initial penetration. The residual indentation of the control specimen was 4.1% and the corresponding figure after the sodium hydroxide test was 9.1%. This proves that the material is only slightly softened under this test and does not deteriorate like linoleum. It falls Well below the 5.0% initial penetration permitted of a covering suitable for use inthose installations below grade and for use on relatively fresh concrete. As heretofore pointed out, linoleum completely deteriorates in 6 hours under such conditions.

In order to further compare resistance of my product with that of commercially avaiable linoleum, I have conducted the so-called wet wear test, which consists essentially of abrading a sample of the material with sand and steel balls for twenty minutes while subjected to a 5% sodium hydroxide solution. My product showed a loss of 1.42% in this test, whereas a commercial linoleum showed 5.46% loss. In the same test extended to 40 minutes, my product showed a loss of 2.46% and the linoleum a loss of 11.9%.

The chart of Figure 4 compares the flexibility of the product of my invention with that of linoleum in accordance with the Tinius-Olsen Stiffness test using a weight of 8/in. pounds on the linoleum sample and 2/in. pounds on the more flexible material of this invention. It will be noted that the break angle on the linoleum was 50 and this is generally the angle at which linoleum of 1A," gauge br'eaks. At that angle the linoleum was supporting about 61.5% of the weight. With my material no break occurred even at the top of the scale; namely, 90. and with the sample supporting 85% of the weight. As a matter of fact, no surface cracks were observed at 90. This establishes that the composition oil my invention is more flexible. gauge for gauge, than linoleum.

Figure compares the initial penetration of linoleum and my composition upon aging. These tests were made with conditions of 70 F. and 65% relative humidity prevailing throughout. The chart indicates that the initial penetration of linoleum increases upon aging, indicating that the product generally softens. This has been determined by other workers in the field to be due to water absorption. The product oi' my invention shows an initial penetration of around 25%, increasing to about 36% over a two-day period and then decreasing to about 28%, maintaining about this initial penetration throughout the duration of the examination; namely, 180 days.

While I have described my invention particularly with reference .to flexible iloor and wall coverings and have compared it with linoleum, my invention is not limited to products of this character but contemplate tiles and other iioor or wall coverings which may be relatively hard and rigid. My invention may be otherwise embodiedand practiced within the scope of the following claims.

I claim:

1. A hard surface :door or wall covering or the like comprising from about 20% to about 40% by weight of a binder composed essentially of from about 55% to about 65% of an alcohol soluble phenol-modiiled coumarone-indene resin having a melting point between 5 C. and 15 C., and from about 35% to about 45% of an alkali-insoluble cellulose ether selected from the group consisting of ethylcellulose and benzylcellulose; 4and from about 60% to about 80% by weight oi illling material.

2. A hard .surface iloor or wall covering or the like comprising a wearing layer having an initial penetration as herein dei'lned of not more than 50% after immersion for 18 hours in a. 2% sodium hydroxide solution and a residual indentation as herein dened of not more than comprising from about 60% to about 80% by weight oi illng material and from about to about 40% by weight of a binder composed essentially of from about 55% to about 65% of an alcohol soluble phenol-modiiled coumarone-indene resin having a melting point between about 5 C. and about 15 C. combined with from about 35% to about 45% of an alkali-insoluble ethylcellulose.

3. A hard surface door or wall covering or the like comprising from about 20% to about 40% by weight of a binder composed essentially of from about 55% to about 65% of an alcohol soluble phenol-modified coumarone-indene resin having a melting point between 5 C. and 15 C.. and from about 35% to about 45% of an alkaliinsoluble ethylcellulose; and from about 60% to about 80% by weight of illling material.

4. A hard surface iloor or wall covering or the like comprising from about 20% to about 40% by weight of a binder composed essentially of from about 55% t0 about 65% of an alcohol soluble phenol-modified coumarone-indene resin having a melting point between 5 C. and 15 C., and from about 35% to about 45% of benzylcellulose; and from about 60% -to about 80% by weight of illing material.

5. A'hard surface floor or wall covering or the like comprising about`% by weight of a, binder composed essentially of from about 55% to about 65% of an alcohol soluble phenol-modified coumarone-indene resin having a melting point between 5 C, and 15 C., and from about 35% to about 45% oi an alkali-insoluble cellulose ether selected from the group consisting of ethylcellulose and benzylcellulose; and abou-t by weight oi lling material.

6. A door or wall covering or the like compris- .ing about 175 parts by weigh-t of a binder essentially composed of about 125 parts by weight of an alcohol soluble phenol-modified coumaroneindene resin having a melting point between 5 C. and 15 C., and about 75 parts by weight of an alkali-insoluble ethylcellulose; about 485 parts by weight of illling material; and coloring pigments.

7. A hard surface oor or. wall covering or the like comprisin-g from about 20% -to about 40% by weight of a binder composed essentially of y parts by weight of an alcohol soluble phenolmodified coumarone-indene resin having a melting point between 5 C. and 15 C., and about 52 parts by weight of benzylcellulose; and from about 60% to about 80% by weight of filling material.

8. A hard surface floor or wall -covering or the like comprising a wearing layer having an initial penetration as herein defined of not more than 50% after immersion for 18 hours in a 2% sodium hydroxide solution and a residual indentation as herein dened oi. not more than 10% comprising from 'about 60% to about 80% by weight of filling material and from about 20% to about 40% by weight of a binder .composed essentially of from about 55% to about 65% of an alcohol soluble phenol-modified coumarone-indene res'ln having a melting point between about 5 C. and about 15 C. combined with from about 35% to about 45% of an alkali-insoluble ,cellulose ether selected from the group consisting of ethylcellulose and benzylcellulose.

9. A hard surface floor or wall covering or .the like comprising a wearing layer having an initial penetration as herein defined of not more than 50% after immersion for 18 hours in a 2% sodium hydroxide solution and a residual indentation as herein deined of not more than 10% comprising from about 60% to about 80% by wei-ght of illling material and from about 20% `to about 40% by weight of a binder composed essentially of from about-55% to about 65% of an alcohol soluble phenol-modified coumarone-indene resin having a melting point between about 5 C, and about 15 C. combined with from about 35% t0 about 45% of bem'ylccllulwe.

WARREN STUBBLEBINE.

REFERENCES CITED The following references are of record in the ille of this patentz UNITED STATES PATENTS Number Name Date 1,625,416 Li-lienfeld Apr. 19, 1927 2,098,362 Rivkin Nov. 9, 1937 2,145,648 Fawkes et al Jan. 31, 1939 OTHER REFERENCES Lorand, Ind. 8: Eng. Chem., May 1938, pp.-

Certicate of Correction Patent No. 2,457,848. January 4,1949. WARREN STUBBLEBINE It is hereby certified that error appears in the printed specification of the above numbered patent requiring correction as follows:

Column 5, line 56, for the word and after the numeral 6 read to;

and that the said Letters Patent should be read with this correction therein that the same may conform to the record of the case in the Patent Oice.

Signed and sealed this l26th day of April, A. D. 1949.

THOMAS F. MURPHY,

Assistant Oommz'moner 0f Patents.

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