US2292542A - Acceleration of the speed of seasoning of surface covering compositions - Google Patents

Description

Patented Aug. 11, 1942 ,UNITED ST S v Accsmaarion or '1' :PEEn mistress.

me or SURFACE covsamc- COMPQ1- TIONS Donald G. Patterson, Stamford,- Conn., assignorj to American Cyanamid Company, New York, N. Y., a corporation of Maine No Drawing. Application April 26, 1940, Serial No. 331,812

4 Claims. (Cl. 106-264) This invention relates to the acceleration of the rate of curing or seasoning" of surface covering compositions such as floor covering compositions containing siccative binders.

An object of this invention is to provide accelerators for surface covering compositions containing siccative binders which will. cause such compositions to cure more rapidly.

This and other objects are attained by incorporating in a siccative composition which is to be used in a floor covering composition or other surface covering composition a guanamine, i. e., of the probable formula:

Ri\ N/ \N R1 N t J-l .R. R, or the tautomeric forms thereof, wherein R, R1, Ra, Re and R4 may be aliphatic, cycloaliphatic', aralkyl or aryl, or R1, R2, R3 and R4 may be hydrogen, and where at least one of the "R" groups includes at least six aliphatic carbons. Those compounds wherein the R. containing at least six carbon atoms is a branched chain are especially useful.

is placed in a stoving oven through which a current of heated air from about 70 C. to about 90 C. is circulated until the material is completely Thefollowing examples are given by way of il- These substances. .with or without a small proportion of drier, e. g. 0.1% -cobalt naphthenate, are mixed together, e. g., in an internal mixer. The compacted mass which is delivered from the mixer may be disintegrated, as by a set of scratch rolls." which comprises a plurality oi'rolls having 'intermeshing teeth projecting from their surfaces. The resulting material is sheeted on calender rolls or optionally it'may be further mixed and disintegrated and then calendered. The material may be calendered on to burlap or other seasoned," i. e., until the sheet acquires the necessary degree of hardness. Higher or lower temperatures may be used if desirable.

The hardness may be measured by any of the methods generally employed in the manufacture of linoleum. See the Federal Stock Catalogue (U. S. Government Printing Office) section 4, part 5, pages LLL-L-351 et seq. and pages LLL-L-36l et seq., for the method employed herein. The

time required for seasoning"'a 2 mm. sheet of the above composition is about 5 to 6 days.

The resulting seasoned floor or surface covering has about the same strength and flexibility as compositions which do not contain the accel erator. Furthermore, surprisingly enough, the

compositions containing the accelerators have slightly lighter color than the compositions not containing any accelerator and this is to be'compared with the darkening effect which is obtained with many other accelerators. Not only do many of the other accelerators discolor the surfacecovering compositions but, in some instances, they also affect the strengthwand flexibility in such a way as to render the materials commercially-unsatisfactory. The seasoning speed of a 2 mm. sheet of the same mixture as employed in this example which does not contain any lauroguanamine is about 18-20 days. I

Example 2 v Parts by weight Binder I 30 Wood flour 30 Whiting 20 Lithopone s 20 Lauroguanamine 0.3 This composition may be mixed and sheeted according to the procedure 01' Example 1. The sheeted composition seasons in about 4 days and has the same desirable properties as the compositions produced according to Example 1.

The siccative binder utilized in the above ex- I amples is an alkyd resin which has sicca'tive prop- -erties, i. e., a reaction product of fumaric acid with a non-coniugatedterpene(alpha pinene) and triethylene glycol, modified with linseed oil 5 fatty acids. Other similar resins may be used which are drying oil-modified reaction products of maleic or 'fumaric acids with a terpene and a polyhydric alcohol. Other alkyd resins which are modified with drying oils may be used suchas fibrous backing if desired. The sheeted material the phthalic-glyceride resins, the glycol-maleic resins, and mixed resins such as the phthalicfumaric-glycol-glyceride resins. With other types of binders, the "seasoning temperature may be varied appropriately and, of course, the time required may be different. About the same proportional accelerating effect is obtained ,when various siccative binders are employed.

Other binders which may be used are those which are derived from the drying oils and may be made in any convenient well-known manner, such as the method described in British Patent 305,656, or the binders may comprise any of the various alkyd resins having siccative properties. For drying oil binders, linseed oil is preferable for economic reasons but other siccative oils may be used such as, for example, menhaden or fish oil, tung oil, soya-bean oil, perilla oil, oiticica oil, Scheiber oil, sunflower-seed oil, etc. The term siccative oil as used herein is intended to include not only the so-called drying oils but also the so-called semi-drying oils. Furthermore, it is possible to use mixtures of siccative oils with other fatty oils of the non-drying type.

It may be preferable in the manufacture of linoleum to make use of so-called scrim-oil" or shed oil, either alone or fiuxed with rosin or other gums or resins and/or mixed with a proportion of the so-called mechanical oil. Either of these types of oils may be used singly if 'desired.

In the preparation of the siccative oil binders it is customary to use rosin in admixture with the oil although other substances of the same type may be used, e. g., kauri gum, Congo gum, ester gum, abietic acid and its esters, pimaric acid, etc.

Instead of wood flour and/or the whiting and lithopone used in the example, other fillers or pigments may be used. Examples of such fillers are: cork, cellulose pulp, asbestos, cottonwood tree pulp, walnut shell meal, glass fibers, foliated glass, etc. Among the pigments which may be used the following are included: lithopone, barytes, zinc oxide, titanium oxide, chromates, red lead, white lead, malachite green, chrome green, chrome yellow, Prussian blue, iron oxide, etc. Similarly, dyes and lakes may be used if desirable.

It is generally preferable to use driers in the preparation of the binders. The drier is usually added to the binder during the oxidation process and if desirable, additional drier may be added when the binder, fillers, etc., are mixed together. Suitable driers include the oil-soluble salts such as the naphthenates, resinates and linoleates of cobalt, lead, manganese, zinc and chromium. Only a small proportion of these dries based on the siccative oil content is generally sufficient, e. g., about 0.005 1%, although larger proportions may be used as expedient. Obviously various mixtures of driers may be used.

The term seasoning" as applied to linoleum compositions indicates the process of curing by heating or equivalent treatment to polymerize and/or oxidize the composition to a stage wherein the floor covering is sufliciently hard and resistant to abrasion to be suitable for its intended purpose and yet is still sufficiently flexible to permit the usual bending and rolling required of linoleum. The term maturing is similarly used.

Other accelerators which may be used include: ethyl-n-butyl acetoguanamine, heptoguanamine (CcHi3C:N3(NH2) 2) 2 (a-ethyl-n-amyl) -4-butylamino-G-amino-1,3,5-triazine, di-n-propyl acetoguanamine, methyl isoamyl acetoguanamine, methyl-n-hexyl acetoguanamine, p, p-di-n-propioguanamine, diisobutyl acetoguanamine, namyl-n-heptyl acetoguanamine, di-n-heptyl acetoguanamine, di-n-octyl acetoguanamine, etc.

Obviously mixtures of any of these or mixtures containing lauroguanamine may be utilized in the same way as the single compounds. In some instances, my accelerators may also improve the alkali resistance.

I have found that only a small proportion of these accelerators is generally sufficient, e. g., 0.1- 5% of the siccative composition, but obviously smaller or larger proportions may be used if desirable.

My accelerators are preferably added during the mixing of the binder with the fillers, etc., although they may be added before or during the oxidation of the binder. If my accelerators are added before or during the oxidation they may inhibit somewhat the gelation of the siccative binder. It is to be noted, however, that after gelation my accelerators speed up the curing of the siccative composition.

Obviously many modifications in the processes and compositions described above may be made without departing from the spirit and scope of the invention as defined in the appended claims.

I claim:

I. In a process of curing a surface covering composition including a siccative material selected from the group consisting of drying oils and drying oil modified polyhydric alcohol-polybasic acid resins, the step which comprises adding to such a composition a 'guanamine having a substituent group containing at least six carbon atoms.

2. In a process of curing a surface covering composition including a siccative material selected from the group consisting of drying oils and drying oil modified polyhydric alcohol-polybasic acid resins, the step which comprises adding to such a composition lauroguanamine.

3. In a process of curing a surface covering composition including a siccative material selected from the group consisting of drying oils and drying oil modified polyhydric alcohol-polybasic acid resins, the step which comprises adding to such ,a composition ethyl-n-butyl acetoguanamine.

4. In a process of curing a surface covering composition including a siccative material selected from the group consisting of drying oils and drying oil modified polyhydric alcohol-polybasic acid resins, the step yvhich comprises adding to such a composition 2(-ethyl-n-amyl)-4- butyl-amino-6-amino-1,3,5-triazine.

DONALD G. PATTERSON.