US1790494A

US1790494A - And benjamin h

Info

Publication number: US1790494A
Authority: US
Publication date: 1931-01-27
Anticipated expiration: 1948-01-27

Description

Jan. 27, 1931. R. H. ADAMS ET AL METHOD OF MKING LINSEED OIL Filed July 3, 1925 2 Sheets-Sheet 1 1Min FIFA-'L Lik,

ATTORNEYS.

Jan. 27, 1931. R. H. ADAMsET AL 1,790,494

' IETHOD 0F MAKING LINSEED OIL Filed July 3, 1925 2 Sheets-Sheet 2 l an Patented Jan. 2.7, 1931 UNIT-En STATI-:se

PATENT y OFFICE ROBERT n. ADAMS, or CmEENwICH,r CONNECTICUT, AND BENJAMIN n. THUBNAN, or TUCxAHoE, NEW Yonx, assleNoEs To GOLD DUST CORPORATION, or NEW Yonx,

N'. Y., CORPORATION 0F NEW JERSEY METHOD OF MARIN G LINSEED OIL'- Application led July 8, 1925. Serial No. 41,275.

Our invention relates to method of making linseed oil. y

Amongfthe many uses to which linseed oil is put in the arts are. two, namely, for varvery high-grade product. The ideal oil for these purposes must be 'of light color and is preferably brilliant without any bloom.

Such an oil must also be free from vhat is v '10 known in the art as break when heated to a temperature substantially higher thlan525 F. or when cooled to say 32 F. These breaks in the ordinary oil are-.evidenced by a precipitate which will not be re-dissolved upon cooling from the higher temperature or upon warming from th lower temperature. The presence of these precipitates in the oils as heretofore made, makes it necessary for the varnish or other paint maker to age and filter 2o the oil before using it. The ideal oil shouldv a high viscosity and should have quick body-A ing` nropertiesfwithwhich a larger amount ofthinner'ma-v vlee used than oils as lhereto fore made. Such an oil should yalso have a low phosphorus content, preferably less than one tWb-thousandth-of one percent. The low phosphorus content assures the formation'of v .phosphatides during the process of manufacturing products in which the oilv is used. Such an oil should also be of such character that upon heat bleaching the color will be suiliciently light for use in the' manufacture of Varmsh or m Zmc or lead grmdmg' terial in storage, as well as vthe storage space Preferably there should be no necessity for refining the oil bythe use of caustics, acids,

or other chemicals.

Linseed oil as heretofore made has had certain defects which it has been impossible to overcome prior to our invention. Two of the greatest defects have been the color and the` breaks uponheating to 525 F. or higher, and upon cooling to 70 F. or lower. So far as we are advised no one prior to our invention has disclosed how these defects maybe overcome without at the same time creating other defects somewhat less objectionable, but

- oil.

Efforts have been made heretofore to over- .come the objectionable color of the oil by 3 nilshes and zinc grinding which require ay treating the same with various chemicals, such as alkalies, acids, and others, and while this treatment hasbeensuccessful to a certain extent as to color, these .chemicals have so affected the structure or composition of the oil that the oil breaks whencooled, as above explained. The precipitate resulting fromrthe breaks renders it necessary for the consumer of the 'oil to allow the same to remain in storage ordinarily for a period of six months. During this period the temperature of the oil changes according to the seasons and the precipitate settles in the barrels or other containers. When it is desired to use the oil it is then passed through a filter to remove this precipitate and clarify the oil. If it were attempted to use the oil before this aging period, these precipitates would be formed in the oil after the same had been made into varnish or other paints with the result that the paint or varnish would be objectionable and in fact unusable on high-class jobs. Itthe-refore becomes necessary that the oil be stored' to allow the precipitate'to form and settle.

4Some varnish manufacturers have installed -refrigerating apparatus to .carry the oil and other equipmentnecessary therefor. The art has therefore been seeking for some time a solution of this diiiiculty which will relieve it of the dilemma of either storing the oil or of using the same withthe chance that the product made therefrom will be defective because lof the precipitated matter. 'We have made certain discoveries and have devised a process of making a linseed oil free from all the defects above set forth and an oil which is superior to the best aged oil exist-l ing heretofore and an oil which may be used immediately upon production without the V100 necessity for any chemical treatment whatever, and at a lower cost than the best oils as heretofore made.

We have discovered that one of the chief causes of defects to the oil as heretofore made i's the action of the constituents of the foreign matter which is invariably mixed with the flaxseed from which the oil is extracted. This foreign material is usually designated as dockageand consists of seeds of wild mustard, foxtail, vetch, white mustard, false flax, pig- Weed, clover and grass; also dust, grit` chaff, etc. Of course this doekage Willcontain other material and seeds of other plants dependino upon the section of the country or world 2from which the seeds are gathered. Another substantial cause of the defects in the oil as heretofore made, was that of' improperly controlled heat during the extraction of the oil from the seeds. We have discovered that if thoroughly cleanfiaxseeds are treated as heretofore wherein the temperature is not limited to below about 11.0 F., the resulting oil has most of the defects above mentioned. One of the chief defects is the break uponvheating. On the other hand, it makes no difference what method is used to extract the oil from the seed, if the seeds have not been ,previously cleaned, the above-mentioned defects will appear.

Our new process consists in first cleaning the seeds of dockage so that there will'remain in the seeds preferably not`more than 1% to 11/270, preferably the former, of dockage. These seeds are then placed in an expeller and the oil expelled therefrom by cold pressing.A

That is to say, the expulsion of the oil is so regulated that the temperature of the oil running from the screen to the drip-pan is between 90 and 100 degrees F. Ordinarily this operation results in the expulsion of about. 45 to 50% of the oil content of the seeds Within thel temperature range above given. The cake .from which this oil has been expelled is then treated by an hydraulic press operation in any known Way to remove the balance of the oil. The oil coming from the expellers may contain slight traces of moisture and fine particles of meal. In order to remove this material a. quantity of the oil is run into and fills a tank of about five to six barrels capacity. To this about 100 pounds of diatomaceous earth is added and the mixture is thoroughly agitated with air. This mixture is then run into a filter press. This small quantit)7 mixed with the diatomaceous earth causes the formation of a filter layer on the filter units and then a lar'ge quantity of the untreated oil may be run throughlthe filters, which assures a very clear and brilliant oil. This oil after filtering shows about .60 acid number. color 50 yellow, 5.3 red. This oil as it comes from the filter has many uses and is particularly useful in the manufacture of varnish and is equal in color and other properties to the best varnish oil on the market'which has been chemically treated and bleached. This oil is given in the table below as TA oil.

The oil from the filter may be treated in a very simple manner, that isf-to say, by heat oil described at the beginning of this specification, having all of the qualities there mentioned without any defects, and in the table below is designated as P. M. P. oil.

We have noted that When'oil made by ordinary methods is chilled to 60 F. or lower a cloudiness sometimes appears'and does not disappear until the oil is at a temperature higher than that at which tlfe lcloudiness appeared. But with our oil a cloudiness does not appear until the temperature is 32 F.

"or lower. When a cloudiness appears, it will disappear before the temperature rises to 48 F., indicating that any suspended matter (suchas glycerides crystallized out) caused by the chilling is soluble in the oil at the teinperature of 48 F. or lower.

This bleached oil has a third use and that is that of makingslight fatty acids. These fatty acids-are usually used for makingdriers or salts of drier metals. They are also used for increasing the acid content of any oil used in either zinc-grinding or lead-grinding. Such acids, as made from ordinary linseed oil, either raw or refined, have the great disadvantage of being of a dark color. This is objectionable ifit is desired to use the acids to increase the acid content of a grinding 011, because of a tendency to discolor the product. By employing the bleached oil of our process fatty acid may be made of light color. When used to increase the acid content of an oil, thesefatty acids may be merely added to rthe oil without treating the total quantity of oil as is usually done by the addition of sulphuric acid, heating and bleaching, which operation obviously consumes considerable time, and is rather expensive. Even if this expensive method is used, the resulting oil is many times darker in color than that made from the use of fatty acids which were made from our bleached oil.

tirely free from suspended colloidal matter` or precipitates which are not readily soluble 'in the material upon change ot' temperature:v the material does not break when heated to a high /t/emperatureor cooled to a low temperature;- has a high viscosity and quick bodying properties; requires no refining by chemicals 4and therefore contains substantially all of its {atural constituents; has a lowphosphorus content; will produce fatty acids of unusually light color and may be used as a varnish oil or as a grinding oil in the production of the highest grade paint products.

In the accompanying drawings, we have indicated in: Fig. 1 a fiow sheet givingl a diagrammatic representation of apparatus. which we have used in the process above dethis apparatus'is by no means vthe only apparatus which may be -used in our process,

but that Yit is merely representative.- We have sh wn in Fig. 2 an enlarged view of 1a seed cleaning machine somewhat in detai I' In Fig. 3 we have shown a view of' the ex- J peller on a larger scale than 'thatshown in Fig. 1.

Our invention will be better understood by reading the' following description of the drawings. forming a part thereof.

Referring to Fig. 1, the apparatus consistsl of a bin l for seed storage.` The seeds are conducted from the bin 1 to the seed cleaners 2, 3 and 4. In treating flaxseed we have found I what is known in the trade as a No.8 Monitor cleaner, made by the Huntley Manufacturing, Company of Silver Creek, N. Y., very effec#vv tive for our purpose. The cleaners 2 and 3 are of the type above indicated and each is 40 provided w1th a 16x21/2 inch wire screen and a 4/64V ofan inch perforated metal screen for mustard seed fraction ofthe dockage. By running the seed over these cleaners the dockage is reduced to about 1.6 per cent. The

4 5 cleaner 4 is what is known in the trade as a No. 6 Monitor` cleaner. This cleaner4 is provided with a mustard screen made up of a.

metal plate perforated to 4/64 of an inch.

t When the seeds are run over this cleaner they,

are cleaned of dockage down to about 1 per cent'or less.

Connected with each ofthe cleaners above described is a dust collector 5, 6 and 7, respectively. After the seed has passed over these three cleaners it is conveyed into a Y hopper 8. The rough dockage is discharged at 9 and the mustard seed fraction of the..

J dockage at 10. v

The clean seeds are' conveyed fro' 1 the hopper 8 into the cracking or fiaking r achine 11'.

(This is a two-high roll machine wi h the rolls so adjusted as to just fiake or crack the hulls without grinding the hulls with the meats. This machine is driven at a speed ofabout 6;.y 180 R. P. M. andis provided with means for adjusting the rolls to regulate the crackin From this machine the cracked or flaked see s are delivered to the mixer 12 in which moisture is mixed with the seeds tothe extent of about-3 per cent. An agitating means 13 is 70' shown for insuring a thorough mixing.. Thev seeds mixed with this moisture areconducted by screw conveyor 14 to the expellers. The pressingequipment consists of a plate press 15, a box press-16 and a standard expeller 17. 75 By ordinary manipulation these pressers are operated so as to iex elfrom the seeds about 45 to 50 per cent o the oil without raising the temperature of the oil as it leaves the expellers to a point higher than 90 to 110 F; The oilis conveyed from the expellers to a,

t scale tank 18 where the oil is weighed. Five scribed. .We wish it to be understood that with about 100, pounds of a certain filter aid,

. such as diatomaceous earth. The oil and filter aid are thoroughly mixed by air agitation and the mixture is then run into the filter press 20, whereupon the' filter aid forms a coating on the filter elements, thus assuring a co1 plete filtering of the oil which is later r nA through. From the filter press the oilis runinto testing tanks 21 and 22 and is there tested for .quality before being delivered to the storage tank 23. z

The test of thev oil in the tanks 21 and 22 consists in'removing a sample from the tank and testing the acid number and the color of the oil., In our operation the .acid number runs between .58 and .6 and the color from about 50 yellowand 7 red to about -35 yellow, 57.35 red. The color measurements herein given were determined by the Lovibond colorimeter with 5% inch columr and used inthe customary manner.

. The 'oil that is delivered to the tank 23- 'has many uses, as explained in the first part 'of this specification, but for many purposes we find it advisable to further treat the oil by passing it into the bleaching tank 24,. in which is placed an agitator 25. A steam pipe 26 is placed in the bleach tank and by means of steam the temperature of the oil in the tank 24 may be controlled to any desired point. We prefer to maintain the -temperature 1n the tank 24 at about 180 F.

We prefer to add to the oil in the tank 24 about 31/2 per cent fullers earth and of 1 per cent of a suitable carbon bleaching material.v After the addition ofthe earth and` the bleaching material the oil is pumped through the filter press 27. At the beginning of the operation it is customary to return the oil from the filter press to the bleaching tank nntil a sufficient bed or cake of filter material is built up on the press units. After the filter press is properly prepared the oil is run continuously from the filter press into a storage tank' 28. Theoil comigfrom the filter press 130 Y 27 has a color ranging from about 10 yellow and 1 red, to about 20 yellow and 2 red, and an acid number ofabout .5.

We have shown in Fig. 2 a somewhat more detailed view of the seed cleaning machine. This machine per se forms no part of our invention and we therefore do not deem it necessary to fully illustrate and describe the same. The machine consists of a framework 29 supporting a series of

screens

30, 31, 32, 33. These screens are reciprocated by eccentrics 34 and 35 on a shaft 36. The material .to be cleaned is introduced through the receptacle 37 at one end of the machine or receptacle 38 at the other, or bothat the same time. The foreign matter is removed by means of the fan 29 and the cleaned flax seeds are delivered at 40. The mustard seeds-are delivered at 41, and the screenings at 42. This machine is well known in the art and its operation is thoroughly familiar to those acquainted with the cleaning of axseed..

In Fig. 3 we have shown a standard expeller which is operated by motor 43 and acts to expel the oil from the cracked flaxseed by compressing the seed between the plates 44. The oil is delivered at 45 and the cake or solid matter may be discharged at 46 from the expeller in a well-known manner. This machine is'also Well known to those skilled in the art and its construction and operation need no further description.

The following table gives the ranges of values of the various physical characteristics of crude oil made in the ordinary way and of the oil as it comes from the tank 23 (TA oil) and ofthe oil in the tank 28 P. M. P. 011). Oil s Raw Color 300 yellow, 22 red Acld No 0.6 to 4.0 Viscosity 11/2 seconds Iodine No 180 to 198 Grav1ty .932 to .934 F. F. A .3% to 2.0% Unsapomfiable matter Not over 1.50%

Oil Color AcidNo. Viscosity Iodine No. Gravity :ey-5.311 TA to .6 to 1 lnesc' 18o zo 198 .932 m .934

10i/ 1R PMP to .6 to 1 llfesc' 180 to 198 .932 to .934

Unsa- Refrac- Bodylng pom- Phosphorus O11 F' F' A' igx rate able content matter TA .3 to .5 1. 4793 1 to 5 hrs. 1.07 Less than 001 PMP 3 to 5 1. 4792 1 to 4 hrs. 76 Less than 002 While we have given detailssuch -as the Achanges may be lnade and satisfactory results produced, but we have found that the method above described in detail is the preferred commercial method and that the product identified above is entirly suitable for all commercial purposes.

Throughout the specification and claims the term viscosity and the values thereof given or indicated, are determined by the bubble method, as follows: The instrulnent consists of a glass tube 6 long by in diameter. The tube is sealed at one end and is made in the form of a homeopathic vial so that it can be almost filled with oil or other material and Sealed at the open end with a cork stopper. The tube is filled with oil or other material to such an extent that when the stopper is inserted the air bubble when allowed to flow along the side of the tube is 1/3 the diameter of the tube, i. e. it is 1A, in diameter. The viscosity is determined by first bringing the air bubble completely to method of treatment to a slight degree depending upon the character of the seed used and the section of the country or world from which the seeds came, but in view of the foregoing disclosure,y we believe that those skilled in the art can easily and readily adapt the process to the treatment of any seeds by very slight experimentation.

We claim:

1. The method of extracting linseed oil which consists in cleaning the whole uncracked axseed to a maximum of about 1.5% dockage and pressing the oil from the cracked flaXseed while limiting the upper temperature of the oil below F.

2. The method of extracting linseed oil which consists in cleaning the whole unmg su stantially 110 F.

R. H.. ADAMS. BENJAMIN'H. THURMAN.