US3013960A

US3013960A - Production of dairy wax and low pour point lubricating oils

Info

Publication number: US3013960A
Application number: US831967A
Authority: US
Inventors: William N Axe; Bruce C Benedict
Original assignee: Phillips Petroleum Co
Current assignee: Phillips Petroleum Co
Priority date: 1959-08-06
Filing date: 1959-08-06
Publication date: 1961-12-19
Anticipated expiration: 1978-12-19

Description

Dec. 19, 1961 w. N. AXE ErAL PRODUCTION OF DAIRY WAX AND LOW POUR POINT LUBRICATING OILS Filed Aug. 6. 1959 2 Sheets-Sheet 1 Dec. 19, 1961 w. N. AXE ETAL PRODUCTION OF' DAIRY WAX AND LOW POUR POINT LUBRICATING OILS Filed Aug. 6. 1959 2 Sheets-Sheet 2 United States Patent Office 3,013,960 Patented Dec. 19, 1961 3,013,960 PRODUCTION OF DAlRY WAX AND LOW POUR POINT LUBRICATlNG OlLS William N. Axe and Bruce C. Benedict, Bartlesville, Okla.,

assignors to Phillips Petroleum Company, a corporation of Delaware Filed Aug. 6, 1959, Ser. No. 831,967 9 Claims. (Cl. 208--36) This invention relates to a process for the production of a dairy wax. In another of its aspects, the invention relates to a process for the production of a low pour point lubricating oil. in a further aspect of the invention, it relates to the production of a dairy wax and/or a low pour point lubricating oil from a crude oil by topping the crude oil to remove gasoline and kerosene, ya gas oil fraction, and an unvaporized distillation residue, flashing said residue at reduced pressure to recover additional gas oil, viscosity-breaking residue from the vacuum hashing, thus producing additional gas oil and deasphalting the residue, combining the gas oil and a portion of distillation residue, catalytically cracking said combined oil, obtaining a gas oil fraction, solvent-extracting said gas oil fraction obtaining a parafnic extract, distilling said paraliin'ic extract to remove a heart cut therefrom, as later defined herein, d-ewaxing said heart cut to obtain said dairy wax and recovering a low pour point lubricating oil from the oil .remaining after the dairy wax has been removed. ln a specific embodiment of the invention, the effluent from the cracking step is distilled and a heavy cycle oil fraction is extracted with liquid sulfur dioxide and fractionated. rThe heart cut obtained according to the invention is cooled, a solvent added, and a wax product separated. After removal of wax and solvent constituents, the oil remaining is treated to recover the low pour point oil by further chilling and solvent and wax separation therefrom.

There are presently being used certain paraffin waxes in large amounts for paper and other containers for milk and other dairy products. These waxes are, therefore, known as dairy waxes. of about 120 to about 135 1F.

lt is known that waxes which are contained in crude oils, possess a `wide range of melting points. Thus, ordinary crude oils contain low and high melting pointwaxes and these include microcrystalline waxes. Thus, many crude oils contain parailin fractions of high melting point and having a Wax-like character. This waxy product is often associated with the lubricating oil fractions separated from these crudes, and is extremely detrimental These waxes melt in the range c therein because it adversely aiects the low temperature properties of the lubricating oil, i.e., the lubricating oil has a high pour point. It has been the practice, therefore, to remove this wax from the lube oil fraction, and, of course, the wax so removed and collected has a certain commercial value.

In order to produce dairy waxes which are usually liexible coating waxes, in large quantities, economically and at a better price to the consumer, it is necessary to find a modus operandi which avoids the production of undesired amounts of waxes melting substantially above about 135 F. and microcrystalline waxes which are also high melting point waxes.

rThe production of low pour point lube oils, that is, lube oils which possess good lubricating and flow properties at low temperatures, can only be obtained with crude oil starting materials by treatment resulting in conditioning of the various segments or fractions of the oil and then dewaxing the same when such a fraction or fractions are so conditioned. Thus, it is important to produce a maximum quantity of low pour point oil with 2 a minimum of cost from an ordinary crude 4oil and this can be done only if a combination of steps can be devised in which each step in the combination, so to speak, preconditions the stock in said step for ensuing operations in such a manner that in said operations maximum beneficial results are more economically obtained.

This invention has as one of its principal and important objects the provision of a combination of interrelated steps, modified to yield improved quantities and quality of so-called dairy waxes and low pour point lubricating oils, in an art in which the vast knowledge available and the great many teachings make it extremely diicult for one skilled in the art, in a reasonable time, if at all, to develop by application of routine skill a reasonably acceptable combination ot' steps to yield improved amounts of dairy wax and/or a low pour point lubricating oil from a crude oil stock. Thus, a subordinate object of the invention is the provision of general indications to one skilled in the art of how to proceed to obtain maximum yields of a wax in the melting point range of, say, 1Z0-135 F., at the same time obtaining maximum possible yields of valuable low pour point lubricating oils from the crude oil starting material, and this without producing undesirable quantities of high melting .point waxes and ncrocrystalline waxes. As a further object lof the invention, it provides a unitary combination of steps for obtaining dairy waxes and low pour point lubricating oils. Thus, it is aprincipal object of this invention not only to produce a lube oil which is free of detrimental waxy constituents, but to so alter the process technique that a wax is produced predominantly that has characteristics suitable for us-e in the dairy industry as an impregnant for paper containers.

Other aspects, objects and the several advantages of the invention are apparent from a study of this disclosure, the drawing and the appended claims. l

According to the present invention, there is provided a process for the production of dairy wax and a `low pour point lubricating oil which comprises the steps kof (l) Distiiling a wax-bearing crude oil to obtain a gas oil and a. non-vaporized residual oil therefrom;

(2) subjecting a portion of the residual oil to vacuum distillation to recover a heavy gas oil therefrom;

(3) subjecting the remainder of the residual oil, from which the heavy gas oil has been separated, to a viscositybreaking operation under conditions to produce-substantial quantities of gas oil therefrom and to deasphalt `the same;

(4) Recovering the thus-produced substantial quantities of gas oil by vacuum distillation;

(5) Charging said gas oils together Vwith another por- ,tion of said residual oil to a catalytic cracking operation maintained under conditions to :dehydrogenate naphthene's;

(6) Cracking said combination of oils in said catalytic cracking operation to produce essentially substantial quantities of heavy aromatics-containing gas oil containing the elements of said dairy wax and said 'low 'pourpoint oil;

(7) Solvent-extracting said last-mentioned gas oil obtaining a paraiiine ratlinate containing the elements of said dairy wax and the elements of said low pour point lubricating oil;

(8) Distilling said raffinate oil to remove approximately a heart cut fraction therefrom consisting of fractions rcmaining when about 2 to l0 percent bottoms and 40-60 percent overhead had been removed therefrom;

(9) Dewaxing said heart cut fraction to remove therefrom a solvent phase of soft wax and oil;

(l0) Separating the solvent, soft wax 'and oil-'containing phase from a resulting dairy wax-containing phase;

(ll) Removing solvent from said dairy wax-containing phase to recover said dairy wax;

(12) Further dewaxing said solvent, soft wax and oilcontaining wax to recover a soft wax and solvent phase and an oil and solvent phase;

(13) Separating oil and solvent phase from said soft wax and solvent phase; and

(14) Removing solvent from said oil and solvent phase to recover said low pour point lubricating oil.

Still according to the present invention, the utilization of the viscosity-breaking step upon the vacuum reduced crude oil distillation residue not only increases the recoverable elements of dairy wax and/or low pour point lubricating oil which can be recovered elsewhere in the process, but it also enhances the yields and relative proportions of desirable fractions which are obtainable from the catalyst in the catalytic cracking operation, and, therelfore, from the crude oil, which it is to be understood is not merely a simple chemical reaction of carbon to carbon scission but involves, in the presence of the catalyst, various other reactions such as hydrogen transfer, resulting in saturation, saturation by alkylation, some polymerization, isomerization, etc. Therefore, according to the invention, the specific sub-combination of distillation, viscosity-breaking and catalytically cracking, especially as further combined with the ensuing steps to obtain the heart cut of raffinate from which the dairy wax and low pour point lubricating oil are obtained, is, in the now preferred form of the invention, a most important one.

Further, according to the present invention, the removal of the heart cut fraction from a raffinate obtained, as here, from a solvent extraction of a cycle oil or gas oil from a catalytic cracking operation, is also an important feature since it permits the later recovery of a good yield of desirable dairy wax and the low pour point oil, as set forth and described Referring now to the drawings, FIGURE I is a diagrammatic showing of the steps in an embodiment of the present invention. FIGURE II is an elaboration of steps concerned with the treatment of the distillation residue including the vis-breaking operation.

The feed stock employed in the operations described in the drawings is a low wax Mex-Tex crude oil. It will be noted, however, that crude oils such as waxy Texas Panhandle crude, asphaltic West Kansas crude, and Venezuelan crudes are included among the crude oils which can be utilized effectively in the operations of the invention. Blends of such crude oils can also be used. In some instances, the crude will already have been subjected to a topping operation. A method of characterizing feed stocks, as here described, by vacuum flashing, is given in Johnson and Mills, Industrial and Engineering Chemistry, volume 44, page 1624 (July 1952).

Referring now to FIGURE I, crude feedstock fed by pipe 3 is distilled in column 4. A light overhead comprising gasoline and/or kerosene is removed by pipe 5. A gas oil fraction, removed by pipe 6, is passed to catalytic cracking operation 7. A bottoms fraction is withdrawn by pipe 8 and divided, part being charged to the catalytic cracker by pipe 9, and part sent to a deasphalting operation 10, through pipe 11. In the now preferred operation, deasphalting is effected by first vacuum distilling in column 12 and then vis-breaking at a temperature of 750 to 800 F., in coil 13, and finally vacuum fiashing in tower 14. The overheads from both vacuum still 12 and vacuum tiash tower 14 are fed to the catalytic cracker by

pipes

15 and 16, respectively.

The cracked product is distilled in distillation tower 17 to obtain a light cycle oil taken off at 18, a heavy process, in accordance with the invention. Removal of SO2 from the raffinate obtained at 25 is effected in distillation tower 26, and the raffinate passed by pipe 27 into distillation tower 28 is distilled into an overhead fraction 29, approximately 50 percent, a bottoms fraction 30 of approximately five percent, and a heart cut 31. It is this heart cut which is further processed according to the invention. The extract oil from the SO2 unit can be processed for feed-stock for carbon black production since it contains elements or fractions rendering it especially useful for this purpose.

Heart cut 31 is chilled in chiller 32 and conducted to

rotary filters

37, 38 and 39 where a multistage separation of the solid wax is made. The heart cut fraction containing the slurry of wax first enters filter 37. Methylethyl ketone, or other suitable solvent from storage tank 33 is conducted by pipe 34 to chiller 35, then by

pipes

36, 43, 49, 50, and 51 to

wash sprays

45, 46, and 47. As illustrated in FIGURE I, the wax is filtered in three stages with countercurrent flow of added solvent, conducted as follows: fresh solvent is added to each stage in the wash spray and to the slurry feed to the last filtration (by pipe 85); the liquid phase separated from the last stage is used to slurry the feed to the second stage; the liquid phase separated from the second stage filtration is used to dilute the original heart cut feed stream to the first filter stage. if desired, additional solvent from storage can be added to feed stream 40, as shown by dotted line S6.

Wax from the lters, after heating in heater 41, stripping of solvent in distillation tower 42 and clay percolation treatment in tower 77, was found to have a melting point in the range 1Z0-135 F., was colorless and odorless, and well suited for coating paper milk containers.

Oil and solvent phase obtained from the first filter 37 is passed through cooler 58 into filter 59. Oil and solvent from filter 59 passes by pipe 60 and heater 61, in which it is heated to about 450 F., to distillation tower 62 where solvent is removed from this phase at 63. Oil recovered at 64 is clay-treated at 65, at a temperature of 1Z0-180 F., the finished product being recovered at 66. A yield of about 65 percent based on the heart cut size is obtained at 66.

The oil and solvent eiuent from the wax filters is further adjusted for viscosity by addition of methyl ethyl ketone, as described, and then chilled in 5S to a temperature of about 10 F. This precipitates a residue of soft wax, which, when heated to 420 F. and distilled is stripped of solvent in 69, as noted. A yield of 11 percent, based upon the heart cut size, is obtained at 71.

The wax-containing phase from filter 59 is passed via pipe 67 and heater 68 to distillation 69. After removal of solvent at 70, the wax product obtained at 71 is found to be relatively soft with a melting point of approximately 55 F., and is suitable for use in polish formulations, etc.

The oil produced at 66 was found to be very satisfactory as a lubricant, having a viscosity of about 39 SUS at 210 F., API of 33.51-1.

The method of removing the wax from the heart cut oil fraction is conventional. The oil is cooled to a temperature in the range of 25 to 35 F., a supply of methyl ethyl ketone is cooled to this same temperature and used to dilute the oil phase to a viscosity suitable for handling on the filters. Solvent can also be added to successive stages of filtration, as described, and be used to wash the solid wax on the filters. In general, an amount of solvent about 4.4 times the weight of oil is added prior to entering the filters, and another portion is used for wash- Cycle Oil obtained at 19 and a bottoms fraction 20 con- 70 ing the filter cake and further dilution. This solvent is taining catalyst fines. This last fraction is decanted at 21 and the catalyst slurry returned to the cracking step by pipe 22. The decant oil obtained at 23 is combined with the heavy cycle oil in 19 and extracted with liquid SO2 at 24. The light cycle oil is removed from the recovered in succeeding operations and only a small amount need be added as make-up. We prefer to use methyl ethyl ketone as the solvent, although other solvents such as diethyl ketone, methyl n-butyl ketone, methyl isobutyl ketone, methyl n-propyl ketone, acetone-benzol mixture, propane, petroleum naphthas, ethylene dichloride, etc., may be used.

The wax collected in the ltration step, which is shown here as

filters

37, 38 and 39, is melted in heater 41 and the solvent removed by distillation at 42, as noted, and removed by pipe 75. The stripped, molten wax is then passed by pipe 76 over a bed of bauxite or fullers earth in tower 77 at a temperature in the range 120 to 200 F., and preferably 180 F. A yield, based upon the heart cut size, of about 24 percent is obtained at 718.

Referring now to FIGURE II, there is shown in diagrammatic form with suitable legend and operational data, the processing of a Mex-Tex crude oil according to the invention, including, with ampliiication, the distillation of the crude oil, the vacuum distillation or iiashing of the crude oil distillation residue, the vis-breaking operation and the vacuum flashing which are, respectively, 4, 12, 13 and 14 0f FIGURE I. Also, on FIGURE II, there are given, on the respective portions of this iig ure, conditions which are employed in an elaboration of that portion of FIGURE I which is identified in the box defined by the dashed lines 10. The parentheses in FIGURE II include ranges of pressures and temperatures which are within the `scope of the invention.

The additional operational details involved in the invention and in its'several steps can be routinely supplied v.by one skilled in the art in possession of this disclosure Vand will to an extent, as he will understand, depend 'ing oil and the soft wax are given in the following table.

Table l S02 RAFFINATE WAX I. Wax properties:

Melting point, ASTM, F 126 Tensile strength, p.s.i 200 Oxidation stability, minutes 120 II. Oil properties:

Vis at 210 F., SUS 39.5 Vis at 100 F., SUS 97.3 Viscosity index 110 Gravity, API 33.9 Pour point, F Ov Color, ASTM 2 Flash, F 395 III. Soft wax properties:

Vis at 210 F., SUS 39 Vis at 100 F., SUS 87.7 Viscosity index 130 Gravity, API 361.5 Cloud point, F 66 Pour point, F

The following are physical properties of a low pour point oil prepared according to the invention.

EXAMPLE There is charged .2020 b./h. of MexTex crude through pipe 3 into crude distillation unit 4. A topped crude is removed at 8 and 8l b./h. charged through 9 and `6 into catalytic cracker 7. In addition, 442 b./h. of topped 'crude is charged into the vacuum train (see FIGURE II), and 268 b./h. of vacuum gas oil is charged into the catalytic cracker through 15 and 6. 174 b./ h. is charged through vis breaker furnace 13 and into vacuum iiasher 14 from which V149 b./h. is charged through 16 and 6 into catalytic cracker 7. The catalytic cracker is operated to produce from its eifluent by distillation at 17, 76 b./h. light cycle oil 18, 152 b./h.v

heavy cycle oil

19 and 66 b./h. of heavy bottoms 20. The bottoms are charged into a settler 21 yielding 30 b./h. of slurry oil which recycled into the catalytic cracker through pipe 22. 46 b./h. of decant oil from 21 and 152 b./h. of heavy cycle oil are charged into the SO2 extraction unit 24. SO2 is charged to extractor 24 at a rate of 0.7516 barrel SO2 per barrel of charge oil. Temperatures in tower 24 are 98 F. and 95 F. at top and bottom respectively. About 75 percent raffinate and 25 percent extract are obtained. -Raiiinate is charged to distillation column 26 through 25. After SO2 removal, 149 ba-rrels per hour raiiinate oil is passed by pipe 27 togdistillation i 28. (Equivalent to 3,5818 barrels per stream day or 44,- 000 pounds per hour.) Distillation 28 yields 2,300 pounds per hour bottoms at 30, 19,620 pounds overhead at 29, Y

land 22,080 pounds per hour wax distillate at 31. This distillate is passed by way of chiller 32, mixed with 112,- 351 pounds per hour of second stage filtrate from filter 38 obtained by way of pipe 56 and, after cooling to 25 F., a total of 132,213 pounds per hour'is charged into filter 37. 119,961 pounds per hour filtrate from 37 is devvaxed in filter 59. Wax cake from filter 37 is passed by 79 to tank 52 and repulped with filtrate from lter 39,

`per hour charge is fed through 80 into iilter 318 from which filtrate passes to pipe 56 for use as described. Wax from 318, mixed with 106,095 pounds per hour of methyl ethyl ketone totaling 116,007 pounds per hour, is charged through 82 to filter 39. Filtrate from charge at a rate of 108,022 pounds per hour is mixed with wax from filter 318, as described. Wax from iilter 39 at a rate of 9242 pounds per hour is passed to heater 41 and then distilled in column 42, yielding 3,986- pounds per hour methyl ethyl ketone through pipe 75 and 6,006 pounds per hour stripped wax through pipe 76. T his 'wax is percolated through bauxite or an equivalent material at F., yielding 5,708 pounds per hour of fully refined wax at pipe 78. This wax has a very low oil contentl (usually less than 0.5 percent) of good color (about 25y Saybolt), good odor and good taste.

Filtrate from filter 37 is chilled to 10 F. in cooler 58 before it is dewaxed in filter 59, filtrate 'from which passes at 116,939 pounds per hour through heater 61 to distillation 62, overhead from which is 102,156 pounds per hour of methyl ethyl ketone. SAE 10 oil passes by pipe 64 to clay percolation 65 producing iini'shed lubricating oil at 66.

In the following Table III are given processing dat-a which `are applicable to catalytic cracker 7 of FIGURE I.

Table III PROCESSINGr DATA-CATALYTIC CRACKER Reactor Ranges Bed Temperature, F 908 875-025 Top Pressure, p.s.l.g 14.1k 5-20 Oil Charge Temperature, F.: K Fresh Feed Thru Coil... 730 50G-775 Topped Crude 224 20G-400 Reslurry 576 200-600 Space Velocity 1. 8 1-10 Oat/Oil Ratio (Wt.) 3.47 2-10 Catalyst Circulation, Tons/min.. 16. 7 10-40 Catalyst Residence Time, ruin. 9.6 16-4 Injection-Steam to T.C., #/Hr 2, 656 1, 000-5, 000 Stripping Steam, #/Hour 18, O01 9,`00030,000 Injection Steam, #/Hour 17, 229 8, 000-30, 000

Reasonable variation and modification yare possible within the scope of the .foregoing disclosure, drawings and the appended claims to the invention, the essence of which is that there have been provided steps in combination permitting the efficient economical processing of a crude oil to obtain high yields of improved dairy waXes and low pour point oils, the combination including the steps as discussed, and particularly depending upon the treatment of the residual oil from the distillation of the crude oil to remove gasoline and kerosene therefrom, the treatment in the viscosity-breaking operation, as described, the combination of the gas oils and a portion of the residual oil also as described, and the cracking of these oils under conditions to dehydrogenate naphthenes, and the selection of the so-called heart cut fraction followed by the dewaxing and Wax and oil recovery operations, also as described.

We claim:

l. A process for the production of dairy wax and a low pour point lubricating oil which comprises the steps of:

(a) distilling a wax-bearing crude oil to obtain a gas oil and a non-vaporized residual oil therefrom;

(b) subjecting a first portion of the residual oil to vacuum distillation to recover a heavy gas oil therefrom;

(c) subjecting the said first portion of the residual oil, from which the heavy gas oil has been separated, to a viscosity-breaking operation under conditions to produce substantial quantities of gas oil therefrom and to deasphalt the same;

(d) recovering the said substantial quantities of gas oil by vacuum distillation;

(e) charging said gas oils together with another portion of said residual oil to a catalytic cracking operation maintained under conditions to dehydrogenate naphthenes;

(f) cracking the combination of said gas oils and said another portion of said residual oil in said catalytic cracking operation to produce essentially substantial quantities of heavy aromatics containing gas oil containing the elements of said dairy wax and said low pour point oil;

(g) solvent-extracting said last-mentioned gas oil obtaining a parafiinic raflinate containing elements of said dairy wax and the elements of said low pourr point oil;

(h) distilling said raffinate oil to remove approximately a heart cut fraction therefrom consisting of fractions remaining when about 2 to 10 percent bottoms and 40-60 percent overhead have been removed therefrom;

(i) dewaxing said heart cut fraction forming therefrom a solvent phase containing soft wax and oil and a dairy wax-containing phase;

(j) separating the solvent, soft wax and oil containing phase from the said dairy wax-containing phase;

(k) removing solvent from said dairy wax-containing phase to recover said dairy wax;

(l) further dewaxing said solvent soft Wax and oilcontaining phase to recover a soft wax and solvent phase and an oil in solvent phase;

(m) separating oil in solvent phase from said soft wax in solvent phase; and

(n) removing solvent from said oil in solvent phase to recover said low pour point lubricating oil.

2. A process for the production of dairy wax which comprises the steps of:

(d) recovering the said substantial quantities of gas oil by distillation;

(f) cracking the combination of said gas oils and said another portion of said residual oil in said catalytic cracking operation to produce essentially substantial 10 quantities of heavy aromatics containing gas oil containing the elements of said dairy wax;

(g) solvent-extracting said last-mentioned gas oil obtaining a parafinic raffinate containing elements of said dairy wax;

(lz) distilling said raiiinate oil to remove approximately a heart cut fraction therefrom consisting of fractions remaining when about 2 to l0 percent bottoms and 40-60 percent overhead have been removed therefrom;

(j) separating the solvent, soft wax and oil containing phase from the said dairy wax-containing phase; and

(k) removing solvent from said dairy wax-containing phase to recover said dairy wax.

3. A process for the production of dairy wax and a low pour point lubricating oil which comprises the steps of:

(a) cracking a gas oil containing elements of a hard coating dairy wax in a catalytic cracking operation to produce essentially substantial quantities of heavy `aromatica containing gas oil containing the elements of said dairy wax and said low pour point oil;

(b) solvent-extracting said low last-mentioned gas oil obtaining a parainic raflnate containing elements of said dairy wax and the elements of said low pour point oil;

(c) distilling said ranate oil to remove approximately a heart cut fraction therefrom consisting of fractions remaining when about 2 to 10 percent bottoms and 40-60 percent overhead have been removed therefrom;

(d) dewaxing said heart cut fraction forming therefrom a solvent phase containing soft wax and oil and a dairy wax-containing phase;

(e) separating the solvent, soft wax and oil containing phase from the said dairy wax-containing phase;

(f) removing solvent from said dairy wax-containing phase to recover said dairy wax;

(g) further dewaxing said solvent soft wax and oilcontaining phase to recover a soft wax and solvent phase and an oil in solvent phase;

(h) separating oil in solvent phase from said soft wax in solvent phase; and

(i) removing solvent from said oil in solvent phase to recover said low pour point lubricating oil.

4. A process for the production of dairy wax which comprises the steps of:

(a) cracking a gas oil containing elements of a hard coating dairy wax n acatalytic cracking operation to produce essentially substantial quantities of heavy aromatics containing gas oil containing the elements of said dairy wax;

(b) solvent-extracting said low last-mentioned gas oil obtaining a parainic raffinate containing elements of said dairy wax;

(c) distilling said raffinate oil to remove approximately a heart cut fraction therefrom consisting of fractions remaining when about 2 to l0 percent bottoms and 40-60 percent overhead have been removed therefrom;

(e) separating the solvent, soft Wax and oil containing phase from the said dairy wax-containing phase; and

(f) removing solvent from said dairy wax-containing phase to recover said dairy wax.

5. A process for 'the production of dairy wax which comprises ythe steps of:

, (b) subjecting at least a portion of the residual oil, from which a heavy gas oil has been separated, to a viscosity-breaking operation 'under conditions to pro- F'r duce substantial quantities of rgas oil therefrom and to deasphalt the same;

(c) recovering the said substantial quantities of gas oil;

(d) cracking the combination of said gas oils in a catalytic cracking operation to produce essentially substantial quantities of heavy aromatics containing gas oil containing the elements of said dairy wax;

(e) solvent-extracting said low last-mentioned gas oil obtaining a para'inic ra'inate containing elements of said dairy wax;

(f) distilling said raiiinate oilto remove approximately a heart cut fraction therefrom consisting of fractions remaining when about 2 to l0 percent bottoms and 40-60 percent overhead have beenremoved therefrom;

(g) dewaxing said heart cut fraction forming therefrom a solvent phase containing soft wax and oil and la dairy Wax-containing phase;

(h) separating the solvent, soft wax and oil containing phase from the said dairy Wax-containing phase; and

() removing solvent from said dairy wax-containing phase to recover said dairy wax.

6. A process for the production of dairy wax and a low pour point lubricating oil which comprises the steps of:

(a) distilling a wax-bearing crude oil to obtain a gas oil and a non-vaporized residual oil therefrom; (b) lsubjecting at least a portion of the residual oil, from which a heavy gas oil has been separated, to a viscosity-breaking operation under conditions to produce substantial quantities of gas oil therefrom and to deasphalt the same;

(c) recovering the said substantial quantities of gas oil;

(d) cracking the combination of said gas oils in acatalytic cracking operation to produce essentially substantial quantities of heavy -aromatics containing gas oil containing the elements of said dairy wax and said low pour point oil;

(e) solvent-extracting said low last-mentioned gas oil obtaining a parafnic raffinate containing elements of said dairy wax and the ele-ments of said low pour point oil;

(f) distilling said raiinate oil to remove approximately a heart cut fraction therefrom consisting of fractions remaining when abo-ut 2 to l0 percent bottoms and 40-60 percent overhead have been removed therefrom;

(g) dewaxing said heart cut fraction forming therefrom a solvent phase containing soft wax and oil and a dairy wax-containing phase;

(h) separating the solvent, soft wax and oil containing phase from the said dairy wax-containing phase; (i) removing solvent from said dairy wax-containing phase to recover said dairy Wax;

(j) further d-ewaxing said solvent soft Wax land oilcontaining phase to recover a soft wax and solvent phase and an oil in solvent phase;

(k) separating oil in solvent phase from said soft wax in solvent phase; and

(l) removing solvent from said oil in solvent phase to recover said low pour point lubricating oil.

7. A process for the production of dairy wax which comprises the steps of (a) distilling a wax-bearing crude oil to obtain a gas oil and a non-vaporized residual oil therefrom;

(b) subjecting at least a 'portion of the residual oil, from which a heavy gas oil has lbeen separated, to a viscosity-breaking operation under conditions to 'produce substantial quantities of gas oil 'therefrom and to deasphalt the same;

(c) recovering the said substantial quantities of 'gas oil;

(d) charging said gas oils together with another portion of said residual oil to a catalytic cracking operation;

(e) cracking the combination of said gas oils and said another portion of said residual oil in said catalytic cracking operation to produce essentially substantial vquantities of heavy aromatics containing gas oil containing the elements of said .dairy wax;

(f) solvent-extracting said low last-mentioned gas oil obtaining a parainic raflinate containing elements of said dairy wax; i

(g) distilling said raffinate oil to remove approximately a heart cut fraction therefrom consisting of fractions remaining when about 2 to l0 percent bottoms and 40-60 percent overhead have been removed therefrom;

(h) dewaxing said heart cut fraction forming vtherefrom a solvent phase containing soft wax and oil and a dairy vwax-containing phase;

i (i) separating the solvent, soft wax and oilucontaining phase from the said dairy wax-containing'phas'e; and (j) removing solvent from said dairy wax-containing phase to recover said dairy Wax. 8. A process for the production of dairy wax and a low pour point lubricating oil which comprises the steps of:

(b) subjecting at least a portion of the residual oil, from which a heavy gas oil. has been separated, to a viscosity-breaking operation under conditions to produce substantial quantities of gas oil therefrom and to deasphalt the same;

(c) recovering the said substantial quantities of gas oil;

(e) cracking the combination of said gas oils and said another portion of said residual oil in said catalytic cracking operation to produce essentially substantial quantities of heavy aroniatics containing gas oil containing the elements of said dairy wax and said low pour point oil;

(f) solvent-extracting said low last-mentioned gas oil obtaining a parainic ratlinate containing elements of said dairy wax and the elements of said low pour v point lubricating oil;

(g) distilling said rainate oil to remove approximately a heart cut fraction therefrom consisting of fractions remaining when about 2 to l0 percent bottoms and 40-60 percent overhead have been removed therefrom;

(h) dewaxing said heart cut fraction forming therefrom a solvent phase containing soft wax and oil and a dairy wax-containing phase;

(i) separating the solvent, soft wax and oil containing pour point lubricating oil which comprises the steps of:

(b) subjecting a iirst portion of the residual oil to vacuum distillation lto recover a heavy gas oil therefrom;

(e) charging said gas oils together with another portion of said residual oil to a catalytic cracking operation;

(f) cracking the combination of said gas oils and said another portion of said residual oil in said catalytic cracking operation to produce essentially substantial quantities of heavy aromatics containing gas oil con taining the elements of said dairy wax and said low pour point oil;

(g) solvent-extracting said low last-mentioned gas oil obtaining a parafnic ranate containing elements of said dairy Wax and the elements of said low pour point oil;

(h) distilling said ranate oil to remove approximately a heart cut fraction therefrom consisting of fractions remaining when about percent bottoms and 50 percent overhead have been removed therefrom;

(l) further dewaxing said solvent soft wax and oilcontaining phase to recover a softwax and solvent phase and an oil in solvent phase;

(m) separating oil in solvent phase from said soft wax in solvent phase; and

References Cited in the file of this patent UNITED STATES PATENTS 2,258,633 Thiele Oct. 14, 1941 2,260,994 Knowles Oct. 28, 1941 2,345,129 Kuhn -Mar. 28, 1944 2,660,553 Knox Nov. 24, 1953 2,867,583 Holder et al Jan. 6, 1959 2,902,443 Wadley Sept. 1, 1959 2,906,694 Dunlap et al. Sept. 29, 1959 2,914,457 Beavon Nov. 24, 1959

Claims

1. A PROCESS FOR THE PRODUCTION OF DAIRY WAX AND A LOW POUR POINT LUBRICATING OIL WHICH COMPRISES THE STEPS OF: (A) DISTILLING A WAX-BEARING CRUDE OIL TO OBTAIN A GAS OIL AND A NON-VAPORIZED RESIDUAL OIL THEREFROM, (B) SUBJECTING A FIRST PORTION OF THE RESIDUAL OIL TO VACUUM DISTILLATION TO RECOVER A HEAVY GAS OIL THEREFROM, (C) SUBJECTING THE SAID FIRST PORTION OF THE RESIDUAL OIL, FROM WHICH THE HEAVY GAS OIL HAS BEEN SEPARATED, TO A VISCOSITY-BREAKING OPERATION UNDER CONDITIONS TO PRODUCE SUBSTANTIAL QUANTITIES OF GAS OIL THEREFROM AND TO DEASPHALT THE SAME, (D) RECOVERING THE SAID SUBSTANTIAL QUANTITIES OF GAS OIL BY VACUUM DISTILLATION, (E) CHANGING SAID GAS OILS TOGETHER WITH ANOTHER PORTION OF SAID RESIDUAL OIL TO A CATALYTIC CRACKING OPERATION MAINTAINED UNDER CONDITIONS TO DEHYDROGENATE NAPHTHENES, (F) CRACKING THE COMBINATION OF SAID GAS OILS AND SAID ANOTHER PORTION OF SAID RESIDUAL OIL IN SAID CATALYTIC CRACKING OPERATION TO PRODUCE ESSENTIALLY SUBSTANTIAL QUANTITIES OF HEAVY AROMATICS CONTAINING GAS OIL CONTAINING THE ELEMENTS OF SAID DAIRY WAX AND SAID LOW POUR POINT OIL, (G) SOLVENT-EXTRACTING SAID LAST-MENTIONED GAS OIL OBTAINING A PARAFFINIC RAFFINATE CONTAINING ELEMENTS OF SAID DAIRY WAX AND THE ELEMENTS OF SAID LOW POUR POINT OIL, (H) DISTILLING SAID RAFFINATE OIL TO REMOVE APPROXIMATELY A HEART CUT FRACTION THEREFROM CONSISTING OF FRACTIONS REMAINING WHEN ABOUT 2 TO 10 PERCENT BOTTOMS AND 40-60 PERCENT OVERHEAD HAVE BEEN REMOVED THEREFROM, (I) DEWAXING SAID HEART CUT FRACTION FORMING THEREFROM A SOLVENT PHASE CONTAINING SOFT WAX AND OIL AND A DAIRY WAX-CONTAINING PHASE, (J) SEPARATING THE SOLVENT, SOFT WAX AND OIL CONTAINING PHASE FROM THE SAID DAIRY WAX-CONTAINING PHASE, (K) REMOVING SOLVENT FROM SAID DAIRY WAX-CONTAINING PHASE TO RECOVER SAID DAIRY WAX, (L) FURTHER DEWAXING SAID SOLVENT SOFT WAX AND OILCONTAINING PHASE TO RECOVER A SOFT WAX AND SOLVENT PHASE AND AN OIL IN OLVENT PHASE (M) SEPARATING OIL IN SOLVENT PHASE FROM SAID SOFT WAX IN SOLVENT PHASE, AND (N) REMOVING SOLVENT FROM SAID OIL IN SOLVENT PHASE TO RECOVER SAID LOW POUR LUBRICATING OIL.