US1448084A - Method of producing lubricating oils - Google Patents

Description

Mar. 13, 1923. I .l,448,084

' 11 F.(DTT

METHOD 0F PRODUCINQ .T'JUBRICATING OILS Filed May 1, 1920 Patented Mar. 13, 1923.

UNITED STATES PATENT OFFICE.

THOMAS F. GT1, BERKELEY, CALIFORNIA.\

METHOD or PRODUCING LuBRIcA'rmGoILs.

the lubricating distillates or oils in sucha manner as to produce in a single-cycle of operation the light'colored oils required or demanded by the public, and which it is the desire of the manufacturer to supply,

1 but which heretofore has not been accomplished successfully except at a materialincrease in cost. The essential objectsjof the present invention are to produce light colored oils at a materially less expensethan under the former methods employed; to expedite the manufacture of such colored oils;

to successfully produce the desired light colored oils in a single cycle of operation and by so doing materially increasingthe daily output of a plant of given capacity, and todispense with the filtration of the oil through a. filtering medium of fullers earth, and which filtering step is essen-' tial in such previous methods employed and generally followedin all manufacturing plants for the production of light colored oil-s.

ess of treating lubricating distillates or' oils for the production of light color oils, embodied essentially the following steps. First agitating the distillate or oil with sulphuric acid, settling out and withdrawing the sludge produced by the acid re-action; second, a subsequent agitation or spraying with a suitable neutralizing agent, for instance,

sodium hydroxide, a settling out and withdrawal of the waste alkali and possible followed in the order given constitutea single cycle operation, but the lubricating oil so produced was generally of a red colorv Prior to the present invention the. recognized and accepted standard method or'procproducts of reaction; third, washing by agi- 1920. Serial No. 378,094.

and in order to produce the pale or light colored oils in popular demand by the pub.-

lie for gasoline motors, it was required to,

carry the method a step farther, viz': filter the oil so produced through a decolorizing] agent,usually by passing the same through a tank or filter filled with fullers earth.

. Each manufacturer varied as desired the quantity of sulphuric acid used and neutralizi'ng agent employed and equally so the time periods of treatment, but for a, full understanding of said standard method, the

following description is illustrative:

Approximately, seven hundred (700) barrels of lubricating distillatewere placed in 4 an acid-agitator, a conical bottomed vessel having a holding capacity of about one thousandflOOO) barrels. The oil was then agitated in the presence of about seventytwo :hundred (7200) pounds 'of 98% sulphurio acid added thereto, by means of com pressed air for a period of approximately thirty (30) minutes. After agitation settlingwas allowed for approximately two hours and the sludge formed drawn. The oil-was then subjected to a secondagitation with an additional ninety-seven hundred (9700) pounds of sulphuric acid for a period of about thirty minutes, settling allowed for sixteen hours and the sludge drawn off as before. Agitation was again resorted to and an additional thirty two hundred (320 pounds of acid was added and, at the expiration of thirty minutes 9 blowing with acid. water. was sprayed over the surface of theoilv This, water is known as coking water and its addition during agitation was tocollect and agglomerate the very fine particles 'of sludge formed by the action of the acid on the oil, into particles ofsuch size as to settle out fairly easily. .No coking medium was required during the two first agitations, due to the fact that the first two increments of acid resulted in the formation of a sludge not so finely divided and which consequently settled out with ease. Following the application of the coking medium, settling was allowed for one hour, the sludge drawn off and the oil transferred from the acid agitator into an alkali agitator, similar in construction to the acid agitator. A hot solutionof sodium hydroxide was sprayed onto the oil until about 160 barrels had been added and settling was then allowed for two hours. The waste alkali and ossible reaction products were drawn and fresh alkali added until the oil was thoroughly neutralized. The alkali was settled out as well as possibleby standing about 16 hours and then drawn off. The oil was then washed by spraying on hot water to remove any traces of alkali and the water settled out as perfectly as possible and drawn ofl' However, mere settlin not being sufficient' to. remove all traces o moisture, the

Oil a e h n transferred t a th s p lbwi-li'ctan'gulir. fin known as the blow w p'a oil was'heate'd 3 mean .of closed ste m coils and com;

pressedair pissed through it until the Oil was perfectly bright andfree from moisture. The resulting oil was generall of aired coleraiid'in order to produce t e pale for ..light colored oils in popular demand for gasolineiniotors, it was necessary to filter this oil thrjough a tank filled with fnllers earth, whi'ch isafdecoloriz'ing agent.

was e slow and expensive process and U at Various times t w s endeavored to produce light colored .oils by increasing the amount of acid in the chemical treatment However, results were not encouragin and, in fact, the larger amounts or acif used seemed to result in an even darkerred oil in th l wrp i n en emp oy the larger vamounts of acid, additions were always made in three increments, although the relative proportions of th increments were varied, 'One coking water? waszilways used after the last increment of acid. ,Efl'orts were made to get a light colored oil by'using. a larger amount of acid by taking the oil f om the blow-pan and putting it :back in the acid agitator and so subject it to, I a complete additional cycle of chemical treatmentnfl i i As the u al p af w ste give a treat of oil about 120,000 ounds of adder pres ticallyflthirtfy poun s of acidper barrel of oil thee i1. when put through two cycles not 1 'lfleivddm bl he amount 7 of acid, but also of alkali and were, In the second cycle'tlie sludge formed by the action of the l acidwas less in amount than during the first the ,oil being treated with'each alkali wash,

added to the ,cost of thealkali and operating costs, make a two cycle treatment uncommercial, but'I am enabled by my invention to produce a decolorized. .oil economically and in a shorter period of time.

In order to produce the pale or light,

colored oil by a single cycle treatment and at the same time dispense with the use of fullers earth filtration or other de-coloring agent after treatment of the oils in thealkali agitator, I discovered the following method of treatment, which will be readily understood by reference to the accompanying sheet of drawings wherein is represented diagrammatically the movement of the oil through a single cycle treatment.

Theusual' amount of oil, about seven hundred barrels, is placed within the agitator 1 and during agitation si' bjected tothe action of forty thousand pounds of sulphui'ic a'cid,t'he acid being addedin four or five increments. After the first increment of say, eight thousand pounds, the oil is agitated for'fifteen minute's, andsettling allowed for two hours. The slud e is then drawn ofi through the controlled outlet 2 of't'he agitator 1, and a second increment of eight thousand pounds of acid added to the oil and, the same agitated for fifteen minutes, and allowed to settle for approximately sixteen hours before drawing oflt' the sludge- The oil is then subjected to a third agitation with eight thousand pounds of acid for a period f fifteen minutes and durg i' agitation treated with about seven barre. 0f coking water for agglomerating and collecting the small farticj es of sludge con tained there in ands lowed to settle for six hours. The oil i'sthen subjected to two additional agitations, with each there being addd ightfthOusaI-id pounds of acid, the agitation and settling being as before, coking water or other coking agent being spra edjonto the oil during each period of agitation after the adding of the acid. It willbe understood that after each settling period the sludge formed by the acid r act on i r v 0 t, although th s ling between increments of acid is a variable fac tor dep endent on the character of oil to be "treated. After subjecting the oil to the of the series of applications of coking water and withdrawal of the sludge, the

011 then need Ortrwu g formed by reactions of the sulphuric acid is transferred 'to an alkali agitator 3, similar in all respects to'the' agitator 1 and, as common in the art oftrea ting the oil sprayed with a hot solution of sodium hydroxide until about one "hundred and sixty barrels are itddfidflfld; the oil fthen allowed ,toscttIe for about two hours, The waste alkali is drawn oi and alkali added until the oil is theroughly neutralized. vFrom this point on and in faetfrom thetime' oi transference of the oil into the a'llkali agitator, the method is ,the' san ieas that heretofore followed, except'tha't after treatment in the acidagitator the oil is not passed through fullers earth or subjected in any manner to decolo-rizing agents, su'ch'being rendered unnecessary by reason of the factthajt subjecting the oil to with filtration by the removal from within the oil of the sludge formed by the reactions of the sulphuric acid} The severalcoking treatments or multiple-coking employed or utilized in my process permits of an increased amount of sul'-,

' phuric acid being utilized in one cycle of operation. 'lVhile the'use of water asa coking medium is specifically mentioned in the treatment of the oils, it will be understood that water is notessential as the coking medium, inasmuch as a weak solution of sodium hydroxideancl a. Weak acid solution have been utilized by me with success, pro- Vided that the solution of sodium hydroxide is dilute enough to have no appreciable neutralizing effect upon the mixture of oil and acid, and, therefore, by the expression coking medium or coking agents as hereinafter employed, is meant to be understood the utilization of Water or any other permissible solution as the coking medium, but preferably I use Water inasmuch as the use of weak sodium hydroxide or weak acid adds materially to the cost of the process without producing other beneficial result by their use in the place of Water.

The use of the multiple coking employed in the step for eliminating the reaction products of the sulphuric acid is the simplest, cheapest and easiest way for most completely removing the sludge formed in the acid agitator after each increment of acid.

It is essential that multiple coking be utilized in order that the reaction products of the acid employed in connection with one treatment be removed as completely as possible before adding fresh acid, for, otherwise, the increased amount of sulphuric acid tends to oxidize or burn the oil.

While the maximum amount of acid used in the carrying out of my method is generally double that used in the former methods employed for the treatment of the oils, or roughly sixty pounds of acid per barrel of oil treated, yet the amount of acid is adjusted according to the degree of color desired in the finished product, and experience has demonstrated that quite a few of the oils do not require double the amount of acid to be utilized in my single cycle operation, over the quantity of acid employed in the carrying out of the former methods.

While the number and size of the increments of acid employed is not fixed, practical experiments have demonstrated that preferably these should be five in number, and While the coking treatment may be a variable one, the same should never be less than two in number.

Contrary to popular conception, the use of the additional amount of sulphuric acid required in the carrying out of my process does n'ot'result inaj smaller yield of the finished'lubricating oil, for the percentage losses in'this process are no higher than in the former methods employed;

-The invention desired to be protected resides in subjecting the distillates or oils for treatment to a plurality of agitating periods,

each period being followed by a period of settlement and each period of agitation being in the presence of a fixed quantity of sulphuric acid added to the oil and subjecting the oil during certain successive agitating treatment to the application of a coking medium, 'the' coking medium being applied to the oil during thesuccessive agitating periods thereof, and in number the coking treatments of the oil being never less than two, whereby the oil is freed of the sludge formed by the acid reactions, so that when delivered from within the alkali agitator the same is of the light color desired.

It will be understood that the foregoing description does not necessarily represent, and is not intended to represent,- the exact treatment for all oils under the present method invention, inasmuch as the quantity of acid coking material, and the quantity and number of acid increments should be varied in accordance with thecharacter of the oil to be treated or to be obtained.

Having thus described my invent-ion, what I claim as new and desire to protect by Letters Patent is i 1. The method of treating oils for the production of light colored lubricating oils without subjecting the same to the action of a decolorizing agent after the acid treatment thereof, the same consisting in subjecting the oil to successive periods of agitation and settlement, adding a given quantity of sulphuric acid to the oil during each period of agitation, and during a plurality of said successive agitations subjecting the-oil to the action of water for the collecting and separation of the sludge formed by the acid reactions, thence subjecting the oil freed of the sludge to a treatment with an alkali solution.

2. The process of decolorizing oils which consists in mixing acid with an oil by a number of increments, adding water to each oil and acid mixture after more than one of the acid increments, removing acid sludge after each acid increment, then washing with an alkali after removal of the acid sludge resulting from the final acid increment.

3. The process of decolorizing oils which consists in mixing acid with an oil by a number of increments, adding Water to each oil and acid mixture after the first two increments, removing acid sludge after each acid increment, then Washing with an alkali after removal of the acid sludge resulting from the final acid increment.

t. The process of decolorizing oils which consists in mix-iug acid with an oil k five eman d n gw ea h? 1 1:;- -ure af ore t an Qne of th Mi d l rp ments, removing spud sludge after each gcyd increment, then washing with an alkali aftpr ber of increments, adding Water to @3011 oil and acid mixture @fber more'than one oi e i iremen s; zem vingu id slndgg after each ac ncmm nmh n wasbi w th an alkali after removal of the acid 11 e msulting from the final aci d treapment; {be number of acid incrementsbeing ppt lg hgm in and. 3m. umb r of WW a d finn f consists in agiigting a lubricaiil, 011 With sulphuric acid, which aqid 3d 9d 1n .6 cesgive incremgnts, mixing main with the Oil d a d mixtur during the thir an sunwi a i wm ms mo i cupid sludge after eagh ipc rgment, 131.1611 Washm with a alkal aftqr' m va o the 11? lllfl e esulting f m he final id inc meat md d awing alka i w ste ,liquglrs- In m timhy whmfioi I have igned my name to thi spmifimtmn- THOMAS F. .OTT.

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