US1794325A - Victor scholz - Google Patents

Description

Patented Feb. 24, 1931 PATENT OFFICE" vrc'roa scnoILz, or nnrrzre, Grimm, assmnon To run rum art-Ks AGO cnrmrscna FABRIK, or norm, um LnIrzIe, GERMANY PROCESS OI PBEPARIQN' G LINOXYN R MATERIALS SIMILAR '10 Lmom No Drawing. Application filed March 2!, 1929, Serial No. 848,074, and in Germany December 21, 1925.

For the manufacture of linoleum linoxyn is used as a starting body for producing the linoleum cement.

Linoxyn is a consistent polymerized and 5 oxidized linseed'oil the iodine number of which decreases through the process of polymerization and oxidation from 186 to about 50-60. V v

In the manufacture of'linoleum Walton 1o linoxyn is used the most, being prepared by thin oil varnish trickling over cloth in oxidizing-houses in temperatures from 4060 C., so that through flooding the cloth several times daily for six months, a layer of linoxyn w is obtained of about 2 cm. thickness. Because of the inconvenience of this Walton process, efforts have been frequently made to produce linoxyn by a quick oxidation process, of which the Taylor process is the most important. In this latter process heated oilvarnish is blown with air into drum-shaped f vessels provided with an a 'tator which begins to act as soon as the o getting thicker and thicker, commences to resist the passage of air; Taylor linoxyn is a ellow-brown elastic bod which does not 'attam the quality of the Walton linoxyn. In Taylor lino the glycerine group of the linseed-oil is estroyed and is lost in the waste-gases such as.

acrylic acid or similar inferior acids. Taylor linoxyn is not oxidized through so much and melts easier than Walton linoxyn the high fusing point of which renders it preferable for the manufacture of linoleum.

5 It has now been found that excellent linoxyns with high melting points can be produced in a surprisingly simple manner'out of varnishes as well as out of pure linseed oils and that the catal st (lead, manganese,

nickel, cobalt, zinc, tm, cadmium, &c., or the oxides of these, or resinate or linoleate compounds) merely aifects the proportions of solubility of the linoxyns obtained and their melting-points. v

%-2% of catalyst, e. 'litharge or linoleate of lead, is dissolved ing stirred at a moderate temperature of 120250 G. in linseed oil, whereupon it is worked into linoxyn in two stages the first one of which is known 59 in itself.

brown products being kneaded inheatable First stage: In' heatable and coolable, tiltable dishes, troughs, or vessels with outlethood and with or without agitator, pure linseed oil or linseed oil plus 2% of catal st, e. g. 2% of litharge, is blown at a possi ly low temperature (GO-150 C.) with cold or warm air, and during the blowing process the oil-temperature is kept at the same height If possible, e. g. at 100 C. Thus a lassy, tenacious, yellow-brown, lustrous, viscous, bod is formed, which finally tears oif from the oiler-wall, copper and agitator, entirely stopping the passage of air orpermitting it only in the way of occasional head-sized bubbles and with an iodine number of about half that of the linseed oil iodine number, i. e. from 90-95 instead of 186. An increase of temperature leads at best to darker smeary prods .ucts,but no further oxidation takes place. The limit of oxidation of the linseed oil or the like oils with saturated groups is attained by the blowin process. I

It was then ound that these blown linseed oils or half oxidized linoxyns of the Taylor linoxyn kind can be further oxidized and improved in a surprisingly simple manner by means of a second process.

' This second process consists simply in the blown, tenacious, viscous, lustrous, yellowso and coolable, high-shovelled kneading machines with access of air, the process, as regards duration and final product, depending merel on the temperature at which the knea ng takes place. a we The kneadin shovels force and ressair into the knea ed mass oxidizing t e same more and more the blown product losing its lustre, getting dull, becoming lighter in color and turning gradually from yellow-brown into a'yellow-orange u to yellow-white, according to the kind 0 catalyst, and finally dropping into fine loose little crumbs while pungent waste-gases are developing. A tenacious blown oil for example made with 2% of litharge, of yellow-brown color, changes during a three or four hours kneadin process at G. into a fine-crumb lightye low-orange colored linoxyn, while blown oils prepared with other catalysts or pure 10f e. g. such as amides and amines (N unsaturated groups can blown linseed oil, will finally yield yellow to yellow-white crumbly to powdery linox us.

If the kneading process is carried on too long or at too high a temperature, many pungent vapours of inferior acids which very much irritate the eyes are developed, the product becoming almost white, very hot and powdery, and if the'cooling and spreading does not take place quickly, it will carbonize in itself while developing heat.

The kneading of air into blown oil or blown varnish is accom lished slowl even in the cold, i. e. in col unheated neading machines, a-slight heat developing by itself. Through the heating and coolin arrangement of the kneading machine t e conduct of the process can be easily controlled and interrupted when the kneaded linoxyn has assumed the quality which experience has proved to be the most favorable. The knead mg process is generall interrupted when the linoxyn has become ight-colored and of a fine crumb and when pungent va ors are develo ing, and in order to stop rther selfoxi ation, cooling and spreading of the lmeaded linoxyn must take place immediatel II l order to prevent the development of decomposing gases and products during the kneading process, which gases are most of an acidic nature, small quantities of rom to 2% of chemical bases may be add ed to the blowing or kneading oils and oil-mixtures, and it has been found that for this purpose organic bases are especiall suitable,

orNH group-containing bodies such as an line Oll, na hthylamine, urea, or similar bodies.

Recording to the catalyst used, or even without the use of a catalyst in the, blowing process the ready kneaded linoxyn can be adapted in its qualities, especially as regards its melting point and its solubility, to the different purposes. V a

Kneaded lmox can be worked 3121p 111 the usual manner or irectly in the kne mg machine after being finished with res ns or copals to linoleum cement. All that is necessary for this purpose is: to add to the l1- noxyn produced in the kneadm machine and havm become finely crumbe res n and kauri-copa in the proportion of 5 resin and 3 kauri-copal to 25 lmoxyn, the res n and copal being powdered and melted for the direct production of linoleum cementwhich can then be transferred in the known manner with color, wood-meal and cork-meal 1n proparts of pigments, and filling substances, into linoleum ground-mass and thus into linoleum.

Besides linseed oil, other 01lS containing be worked in the same way into tenacious, linoxynlike, polymerized and oxidized bodies, e. g. wood-oil, Hevea-oil, Perilla-oil, sunflower-oil, nut-oil, hemp-oil or mixtures of these with each other or with linseed oil. Finally non-drying oils of the oxy-oleic acid series containin unsaturated groups such as castor-oil by itself or mixed with linseed-oil and similar drying oils, can be blown together and kneaded an transferred into firm-crumby end-products, which are again of variable qualities according to the choice of mixed oils and catalysts. In this way lino'xyns and linoleum-cements of an required elasticity can be produced by the a dition of non-drying oils with unsaturated groups, e. g. castor-oil, to the saturated drying-oils during the blowingand kneading-processes.

According to whether the unmixed or mixed oils are blown or kneaded, or whether a catalyst is introduced into the oils before blowin and kneading or during these processes, t e end-product can be re lated with re ard to cold-resistance, fusibihty and solubi it in different solvents.

Finally, linoxyns can be used also for-the manufacture of soaps, for the sizes ing of canvas, tilts, horseankets, kna sac umbrellas, &c. For thesepurposes t e linoxyns prepared accordin to this invention are saonified with al alies, the soap-solution eing eventually mixed or emulsified with tallow wax, glueor leather-solution or other additions, and on the materials impregnated with the linoxyn soap the insoluble oxy-soap is precipitated with baths of watery su phate or acetate of alumina, which renders the textures waterproof, preserves their full porosity and imparts a velvety touch to them.

Linoxyns especially those made of sebacic acid, mixe with soda, borax or the like saponifying materials dissolved in boilin water, may be used also as bleaching and washing materials,- because during the salinoxyns give ofi oxygen.

While I have described the use of air in treating the oils, it is obvious that the resulting oxidation is-produced b the oxygen content of the air and I there ore claim in some of my claims broadly the use of oxygen.

Claims:

1. A substance which consists of a polymerized and oxidized oil of the type having a molecule with an unsaturated group and which has a fine-crumby, flaky yellowish opaque consistency as a result of a kneading process to which said oil has been subjected d portion of 33 parts of linoleum cement to 66 after Preparatory conversion into a jelly' by oxidation effected. by air blown through the oil at an elevated temperature.

2. The proce'm of manufacturing a linoxyn-like material comprising blowing oxygen through an oil, the molecules of which have unsaturated groups, until it is converted into a viscous body and thenkneading oxygen into said viscous body until it attains a fine, crumby, opaque consistency.

3. The process of menu acturing linoxy'n which comprises blowing oxygen through linseed oil until the latter is converted into a viscous body and subsetuently kneading oxg'gen into/said viscous bo until it attains a ne, crumby, opaque consistency.

4.. In the process claimed in claim 2, adding a catalyzer to the oil before blowing oxygen therethrough.

5. In the process of claim 2 adding a basic material before commencing the kneading operation in quantities sufiicient to prevent the development of acid gases.

6. In the process claimed in claim 2 mp idl coolin the product after it has attained a fiiie, crum y, opaque consistency to prevent continued oxidation and the development of acid gases.

7. The process of manufacturing lino xyn which consists in adding a catal ic compound to linseed oil, blowing air eated to C. through the resulting mixture until the oil has been converted into a viscous bod kneading the air into said viscous body whi e maintaining the temperature of the latter at about 100 C. until it attains a fine, crumby, opaque consistency and then rapidly cooling the material to avoid self-oxidation thereof and the development of acid gases.

In testimony whereof I have signed my name to this specification.

VICTOR SCHOLZ.

mousse verted into a viscous body and then kneading oxygen into said viscous body until it attains a fine, crumby, opague consistency.

3. The process of menu acturing linoxy'n 5 which comprises blowing oxygen through linseed oil until the latter is converted into a viscous body and su uently kneading ox gen lDiSO/Sflld viscous y until it attains a ne, cru'mby, opaque consistency.

9 4.. In the process claimed in claim 2, adding a catalyzer to the oil before blowing oxygen therethrough.

5. In the process of claim 2 adding a basic material before commencing the kneading )5 operation in quantities suflicient to prevent the development of acid gases.

6. In the process claimed in claim 2 rapitll coolin the product after it has attained a fi ne, crum y, opaque consistency to prevent 20 continued oxidation and the development of acid gases.

7. The process of manufacturing linoxyn which consists in adding a catal 'c compound to linseed oil, blowing air eated to 100 0. through the resulting mixture until the oil has been converted into a viscous bod kneading the air into said viscous body whiis maintaining the temperature of the latter at about 100 C. until it attains a fine, crumby,

opaque consistency and then rapidly coolin the material to avoid self-oxidation thereo and the development of acid gases.

In testimony whereof I have signed my name to this specification.

VICTOR scnonz.

CERTIFICATE. OF CORRECTION.

Patent No. 1,794,325. Granted February ;4, 1931, to

vlcron 'scnoLz.

It is hereby certified that the above numbered patent was erroneously issued to the firm "Atlas Ago Chemische Fabrik", as assignee of the entire interest in said invention, whereas said patent should have been issued to the inventor, said Scholz and to the firm Atlas Ago Chemische Fabrik, said firm being assignee of one-half interest only in said invention, as shown by the records of assignments in this office; 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 Office.

Signed and sealed this 29th day of September, A. D. 1931.

' M. J. Moore, (Seal) Acting Commissioner of Patents.

CERTIFICATE OF CORRECTION.

Patent No. 1,794,325. Granted February 1931, to

VICTOR SCHOLZ.

It is hereby certified that the above numbered patent was erroneously issued to the f irm "Atlas Ago Chemische Fabrik", as assignee of the entire interest in said invention, whereas said patent should have been issued to the inventor, said Scholz and to the firm Atlas Ago Chemische Fabrik, said firm being assignee of one-half interest only in said invention, as shown by the records of assignments in this office; and that the said Letters Patent should be read with this correction therein that the same may conform to the record of the ease in the Patent Office.

Signed and sealed this 29th day of September, A. D. 1931.

M. J. Moore, (Seal) Acting Commissioner of Patents.