DE1287241B - Process and device for alkali refining of glycero oils - Google Patents

Description

1 2

The invention relates to a method and affects what at the interface between oil and an apparatus for alkali refining of glyceride alkali is going on.

oil. According to a more recent proposal, oil droplets

The term "glyceride oils" used here. is of substantially uniform size without intended to denote fatty acid glycerides, 5 soak turbulence in an excess of alkali usually carried both solid and liquid. Although in this way the common ones are. Refining losses can be reduced,

Glyceride oils, which are extracted or pressed, have various disadvantages. That's the way it is sen or by other working methods from planting very difficult to get droplets of the same size borrowed or obtained animal raw materials; this requirement is very strict, there den, always contain a larger or smaller smaller droplet in the alkali with smaller Share of free fatty acids. Before these oils at the. · Speed rise as larger and due The manufacture of foodstuffs or foodstuffs uses their small size to get rid of acid more quickly can be ;, the free fatty acids must be the. Once the fatty acid is removed, that takes and change impurities to substantially de-saponification levels. Moreover, it is complete be removed. The oldest and best-known deacidification - avoidance of turbulence or eddying The process of disassociation is very difficult. These factors lead to too alkali refining or 'refinement. This assumption of the loss of saponification. A diminished Driving has the advantage that at the same time a travel distance causes an increase in the content of free Reduction of the oils through absorption in the ao fatty acids formed in the neutralized oil, as larger dripping soap of a number of times that occur in the crude oil to complete neutralization which unwanted substances is caused. This can escape. The occurrence of turbulence can cleaning agents obtained during alkali refining prevent that .Tjppfchert, even of the same size, kung has a great influence on the have the same residence time in the alkali, and subsequent work steps or treatments 35 causes some of the droplets to become one such as bleaching, hardening and excessive saponification. This humiliates Deodorize. In acid removal processes, their size and makes them. · AuGh-more sensitive-to which caustic soda solutions are used: ■, over-turbulence. In addition, the concentration decreases However, it is difficult to saponify Glyce- 'the alkali during' the neutralization, so to prevent rides. In addition, it will always be neutral "30 that a longer path is required for the droplets found the soap solution. This leads to the presence of “a complete fair show at the Eijde der is called Neulrajöl in. the "acid oil", which.M. Treatment_z.u ^ ewy.islen._Bas well..can ge-cleavage of the soap obtained by means of acid hydrolysis, oils give rise to difficulties due to one thing • will soon lead to a reduction in the yield of:! Unsatisfactory coalescents & or refined products oil. In general, acid oils are the ones that flow the droplets at the top of the column Contain 30 to 40% or more of neutral oil, still give.

completely applicable. Neutral oil of proportionately It is a method of neutralizing and

good quality can be obtained from the soap solution can be obtained, however, this is quite costly by alkaline lye in the form of thin and playful and therefore technically unsatisfactory. In 40 wide layers ^ Jängs-jSpiral-.or stairs- or the literature describes different working methods for sheet metal arranged in a pre-zigzag fashion. at been beaten, in order to prevent the oil refining in the case of the well-known process reduce any losses that occur. For example, in a vessel filled with alkaline lye was the use of dilute caustic soda and spreads along the lower surfaces of the in the for neutralization, suggested, however, this --4g vessel in a thin layer to a heightened inclination for soap solution. to BU- \ from, The apparatus for "neutralizing oils according to

formation of emulsions.-Furthermore, "the- ''" this principle can be, for example, round, with the oil

Turning of weaker alkaline compounds, leading sheets form an Archimedean spiral; like soda ash and ammonia and the deacidification the apparatuses can also be square, whereby the or the EntfdfiHing ^: veh Acids-mit HÜfe-NfosZen- 5 * sheets tr ^^ ai-shaped "-u ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥} il be} il met, whereby very short contact times between can.

Oil and alkali solution are used before- When the oil is beaten along an inclined plate. Although these proposed labor “sampled upwards through a stationary mass of alka As a result of some improvement, lischer liquor will remain flowing, as has been found that dieol lossespchb ^ rachtIiSh, ^ -;,. ^ ./■; ..;,; s-aS ^ .NeutraliifatjCinsffekts along, the way .of the oil-Im in general, the acid removal or "* shift can be progressive, from and finally becomes zero, Deacidification as a liquid-liquid extract so that the obtained; Product not the desired tion process are considered, but with a low content of -an-free fatty acid. Disagree Features are present which will produce these ar- rently unsatisfactory results make more difficult. The fatty acids will keep up if instead of a single plate one not extracted by means of a selective solvent, plurality of inclined plates in spiral, staircase but rather into the alkaline solution to form an or zigzag arrangement or in the form of a Soap added. However, in addition to this Er-Archimedean spiral, It was found that the above desired effect of the alkaline solution was undesirable Side reactions. An example of the 65 led disadvantages and deficiencies in particular to the One of the more common side reactions is the saponification of the oil, forming a soap film along its path through the oil the alkaline solution. Furthermore, the refined layer is due to which the oil layer nation or refinement process strongly separates it from the alkali. It now resulted

3 4

Difficulty to place this soap film without undue same during the rest of the process. It Emulsification of the oil in the alkali or that is an essential feature of the process according to Alkali in the oil and without excessive deterioration of the invention that such turbulence, which Soap or excessive use of alkali will result in disruption of continuity or des and would result in an unsustainable connection of the system to 5 connections of the oil flow, remove, is avoided. From this point of view, the

It has now been found that satisfactory angles of the guide plates along which the oil

Results in alkali refining of glyceride oils, gradually flowing upwards, preferably less than

in which these are in the form of thin layers of 20 °, angles below 10 ° particularly

an aqueous alkaline solution are treated, io are preferred. The use of guide plates,

with the oil along the underside of in the alka- which are placed horizontally and on their

Liquid solution arranged solid surfaces flows, the underside spreads the oil, is also in accordance with

according to the invention can be obtained by providing the invention.

Both the oil and the aqueous alkaline solution As indicated above, the alkaline

in the same or opposite "direction con- 15 solution both in countercurrent and in cocurrent

be passed continuously through a plurality of treatment streams with the oil stream. The vote

zones that lead upwards through the solid surfaces of each more functional. Way depends on practical

and laterally limited by guide surfaces and where- considerations depend. To achieve a sufficient

at the transition of the oil from each zone in the neutralization, the oil layer should have a thickness of

next higher under such a sharp change of direction 20 have a few millimeters. In general,

takes place that the oil-alkaline at the interface get good results when the oil throughput

Soap film formed in the solution in each zone breaks off below 10 l / hour / cm width of the oil layer

and is distributed in the alkali solution: and that is achieved, with a suitable flow rate 2 to 5 l / h / cm

Hold neutral oil and the soapy aqueous alkali width or width is. .,,

solution continuously discharges separately. 25 When carrying out the procedure according to

During the treatment according to the invention in the manner described above

the oil and the aqueous alkaline solution are processed with sufficient consideration of the different

a repeatedly redirected path, which requires precautionary measures as mentioned above

If there are a series of echelons separated by a distance, it is found that during the directional

includes, where the; » in _which: takes place way that the ~ 3 ° 'changes in the oil flow. the touch, between

Interface between the .aqueous phase and the "this stream and the aqueous soap layer, which

oil layer at the end of each season in the direction of the oil-formed is interrupted, this being called

ßtroms is interrupted, whereupon the oil and the essential factor for achieving the desired

Alkaline solution is viewed in separate related results. V .. _:

Stream from each "season to the next led 35 ...,. The method according to the invention is based on a

will. '\ "wide variety of crude oils applicable, being even

Preferably, the oil moves in each stage with those which are the same a very high content of layer in the ¹ or have in the opposite free fatty acids, products were obtained .Direction to the "alkaline solution due to their their content of free fatty acids 0, 15% or even lower specific gravity slowly upwards, 40 less was ...-.-.
The presence of a small amount of soap in its direction of flow in the alkaline solution, in such a way as to make it easier to find that the horizontal component of fluidity in the neutralization, and under this face, is essentially on, is caused in intervals to change the oil Zero is lowered while the point, soap and / or other wetting agents can be added to the vertical speed component via an Irish alkali. A small vertical distance prevails, the height of which from sodium chloride or similar electrolytes is at least equal to the distance at which the scales can also be added. The use of the right speed component predominates. That of sodium hydroxide as the alkali is advantageous; Each change of direction is carried out in such a way, but other alkaline agents are also used, that a separation of the oil flow is avoided 50 bar. In general, an alkaline solution is used, although the oil layer turns into a plurality of separate streams during the direction "'" of a concentration from 0.05 to 1.5 times, the range from 0.1 to 0, 8normally broken or divided, whichever is preferred. ;

reunite at the beginning of the next stage. In general, the results favorable in the foregoing will be obtained if, during the given manner, the neutralized oil is completely free of any refining or refining treatment including interference from the flow of the alkali solution. borrowed. Drying, bleaching, deodorization, or This may be conveniently carried out by a physical without an intermediate curing step under _r separation of the flow of the oil and Älkalilauge wörfen. It is also advantageous to be achieved between dieNeütrar · each other "by th one or 60! Ization and further refining a both streams through pipes or chambers separated '*" additional treatment with lye einzuschal ¹ -executes so that a contact between them avoided in order to remove a color and the content of free fatty acids will be reduced further.

The formation of oil globules is where the action can e.g. with a vegetable oil in it Change of direction occurs to be avoided, as they consist of the 65, that with a weak alkali, in case of effectiveness of the refining process, for example, 0.2 η sodium hydroxide solution is stirred, whereupon would. When spheres are formed, the oil layer and the aqueous layer cannot be found by means of centrifuges a coalescence or confluence or decantation can be separated. at

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animal fats, in particular animal fats from below the collecting container to a separate one

low quality, such as sebum, may cause a substantial or special discharge. Fig. 2

higher concentration of alkali may be desirable. shows an expedient arrangement for the implementation

This additional treatment with aqueous alkaline tion of the separation.

a concentration in the range from 0.1 to 4 normal 5 According to FIG. 2 is in a housing 8 with a

up to Snormal or even higher can according to inlet 9, in which the alkaline solution and the

the type of oil being treated. protruding oil layer flows, an oil sump

Various arrangements according to the invention 10 are attached, in which the oil via a dam

are given in the examples below and 11 flows and exits therefrom through an outlet 12,

shown schematically in the drawing. io while the alkali solution through the passage 13

F i g. 1 shows a view of a guide device under the oil sump 10 and then over one

device for use in the upward guidance of the second dam 14 flows into a space 15, which flows with

Oil layer along a gradual path. an outlet 16 is provided.

In Fig. 1 is a long rectangular guide It was indicated above that the baffle plate 1 is provided with side flanges 2, which are 15 plates 4 are substantially rectangular; it is in each case advantageous that the baffle plates are slightly used from the surface which is formed as the lower surface 3 of the plate, or beveled, so that they extend against the free ones. (This surface is hereinafter referred to as the bottom surface of the ends of the baffle plates, the oil layer in its width for the sake of simplicity.). On the other hand, contact 20 chen end, the baffle or baffles by Ausaus the lower surface 3 downward take from one or indenting in its width decreases angle of 2 to 1Ö ^east before the moving-Virtually rectangular baffle or baffles. 4 This impact or guiding become. It is also possible to have an arrangement of stainless steel sheets 4 with downwardly protruding side lugs and flanges 5 with inhibiting or obstacle parts in the vicinity. of the free ends of the baffle plates, in operation the guide plate 1 is under a 35 around the oil layer for its upward flow by the inclination of 2 to 10 ° to the horizontal in an alkaline solution in a number of streams to channel or pipe, preferably of equal- interrupt. Details for the various shaped rectangular cross-sections, attached, versions of these baffles are shown in Fig. 3, the upper wall of which adjoins the plate 1, while to 6 shown.

the lower wall parallel to the upper wall and in Fig. 3 shows a view in the forward direction

there is sufficient distance from this to allow the tapering or narrowing baffle plate 4 a

desired flow of alkali solution and oil through that with a rear projection 17 through which it

To enable tube, and the side walls adjacent to the lower side of the guide plate 1, the

beard to the side flanges 2 are. F i g. Figure 1 shows the flange not shown is attached. The opening

upper wall 6 and the lower wall 1 of such a 35 18 between the baffle plate and its flanges 5,

Rohrs. through which the oil layer flows is unobstructed.

In such an arrangement, the alkaline F i can g- 4 shows a forwardly tapered baffle solution the tube at each end in accordance with the Medi 4 b the opening 18 by teeth 19 behin-demand, either wobbles in opposite or in that breaking or subdividing the oil layer into separate streams in the same direction as the oil through the pipe.

stream, enter. The oil gets into the pipe at Fig-5 shows a baffle plate 4c, which is recessed at 20 lower end near the lower surface 3 and in which, in addition to the flow, in the form of a layer in contact with that nenl9, which the opening 18 obstruct, partially surface upwards along the lower surface, obstructed openings 21 provided by teeth 22 until it passes through the first of the baffles or baffles 4 45 ^Sm ^ ·

is deflected "from which it then to the end of Fig. 6 shows a baffle plate id flowing at 20 ausdes baffle. Then it essentially rises and in which a front flange 23 borrowed vertically through the alkaline solution serves to shut off the forward flow of the oil completely and then continues to flow into contact with the upper surface, whereby openings 24 are provided, surface 3, until it is deflected 50 by the next baffle to separate the oil film into a number of separate, downwardly flowing streams.

Thus it takes an upward movement through the pipe.Instead of creating only openings,

directed, essentially step-wise course, as shown in FIG. 6, for the passage of the oil

in the case of a relatively long, slightly upward direction, in separate currents through the alkaline solution,

Tete slopes with relatively short, in the 55 pipes can be provided for this purpose, so

alternate substantial vertical climbs. that these oil flows are free of interference. on the other hand

While the oil is flowing through the pipe or in addition to it, the impingement or

the flanges 2 prevent the spreading of the oil baffle pipes for the passage of the alkaline pipes

layer in any space between these flan solutions without interfering with the oil flow see; the side walls of the tube and the flanges 5 60. When the flow of an alkaline solution through a

serve a similar purpose. The oil is at the end of the line, which is connected to the guide device of the

this way is equipped by the alkaline solution and of the type specified above, in

the aqueous soap solution, which is in the neutral direction opposite to that of the oil,

sation has been formed, separated This separation is there to avoid an interruption of the oil can can be achieved with concurrent flow by 65 currents at its essentially vertical rise.

If the oil flows over a dam into a collecting container, it is very desirable that the baffle plates

ter can flow from which it drains, while the baffles by some means, for example

alkaline and the soap solution for passage of the type described above, are equipped,

7 8

around the oil layer in a number of contiguous - a more closed or compact arrangement,

interrupting flowing or continuous currents. in which the panels are arranged in a zigzag shape

Instead of one equipped with baffle plates, FIG. 8, which two such guide plates can represent a plurality of simple ones in plates. The guide plates 55 and a separate, upwardly directed line 56 are fastened in a housing 54 of guide plates arranged in right-hand rows, each of which has a square cross-section. At the top of each guide plate, downwardly directed flanges 57 and 58 serve to completely shut off or shut off means for the supply of the oil layer exiting under the plate, at the top of the line, and in the vicinity From the upper end to an area under the plate at the lower end io of each guide plate openings 59 and 60 are seen upstream of the subsequent line together with an inlet to separate the oil film in a number of directions for the supply of the alkaline solution to divide under the oil layer at the lower end of a pipe. Between the flanges 57 and 58 and that out of the upper end thereof and then to the wall of the housing, openings 61 and 62 are provided at the lower end of a preceding conduit to allow the alkaline solution to flow without being seen so that the flow through to allow any line disturbance of the oil flow,
is concurrent, while that of one line alone (as shown in FIG. 8 in FIG. 8) for the passage of the oil in ge-FIG. Figure 7 shows an arrangement of this type. separated currents through the alkaline solution

In Fi g. 7, two inclined conduits 25 and 26 ao pipes are provided for this purpose, so that these

of right-angled cross-section, in each of which oil flows are free from disturbances,

a guide plate 27 is axially attached, each to a further alternative embodiment is shown in FIG

their upper end with devices 28 and 29 with F i g. 9 shown. Here again are a number of

a structure as shown in FIG. 2, for separating guide plates in a zigzag arrangement in FIG

of the oil connected by the alkaline solution. Oil from a housing 63 of rectangular cross-section.

a forward provided with a heating device 31, two of these plates, 64 and 65, being

Storage tank 30 is shown through a pipe 32 to be shown. Tubes 66 and 67 are provided which

the lower end of the conduit 25 and close down through the guide plates 64 and 65

the lower surface of the guide plate 27 by means of below the lower limit of the oil layer

a pump 33 is pumped, with it stretching on its way 30 to a separate lead of the alkaline

through a heat exchanger 34 and a stream to allow dissolution of the oil. This will make the

■ measurement meter is guided. After the passage, the oil begins to move upwards in the form of a layer

the lower surface of the guide plate 27 is caused by separate flows through the openings 68

long it becomes of the alkaline solution through the and 69 between the wall of the housing and the

Separator or separator 28 separated and 35 flanges 70 and 71 at the upper end of the guide

then through a pipe 36 to the lower end plates 64 and 65, these flanges

the line 26 where the same treatment is provided to avoid any disturbance of the oil layer

as repeated on line 25. After by sucking the alkaline solution that passed through

Avoid separation of the alkaline solution through which the tubes 66 and 67 are passed.

Separating device 29 is the oil then through the 40 This arrangement proved to be particularly effective

Pipeline 36 β to a collecting tank 37, the sam.

is equipped with a Heizeinrichung 38 is performed. The total number of guide plates in the

The alkaline solution is obtained from a with a heating F i g. 8 and 9 depends on the arrangements shown

device 40 equipped reservoir 39 by the type of oil to be treated and the desired

a pipe 41 to the lower end of the pipe 45 final content of free fatty acids and, as can be seen,

26 (whereby it flows in the same direction as the oil) also depends on the dimensions of the guide

pumped by means of a pump 42, whereby they are reduced by extension plates.

a heat exchanger 34 and a flow instead of guide plates which is guided in the drawing knife 43. After performing through the type shown, helical or the line 26 and separation of the oil by means of 50 partially conical guide plates using separating device 29, the alkaline solution flows can be det. In addition, horizontally arranged along a pipeline 44 to a buffer vessel 45, nete guide plates can be used, from which it is effected through a pipeline 46 to where the oil flow is then effected by the oil at the lower end of the line 25 by means of a pump 47 one end of the Guide plate is introduced and pumped on, being discharged on its way through the 55 other or distant end of this guide plate heat exchanger 34 and a flow meter 48 which is seduced with flanges. After passing through the line it can be seen in order to avoid the escape of the oil under the guide 25 and separation of the oil through the separation plate at the introduction stage or along the direction 28, the alkaline solution flows through one side of the guide plate.
Line 49 to a collecting vessel 52 which is equipped with a heater 53 if a number of guide plates are used. During the flow these are usually equal to one another, the oil and the alkaline solution in each of the lines, however, a series of guide plates of mutually 25 and 26 being aligned so that the species is also effective. For example, if their general flow is in the opposite direction, an oil with a high free fat content where the oil is first passed through line 25 and then 65 acids (5 percent by weight of the oil or more) raffi through line 26 and is to be drained For example, the Verwenkalische solution can be passed through these lines in a combination of a long horizontal reverse sequence. or inclined guide plate as the first stage and one

909 503/1549

Device according to the in F i g. 8 and 9 above the uppermost one of the panels 73 and separately

Kind be advantageous as a subsequent stage. of which through an oil collection chamber 82 is located

10, 11 and 12 show an embodiment of a cover plate 83. The vessel has an outer shape in which horizontally arranged plates are mounted in a cylindrical container in cover 84 with an inlet pipe 85 for the alkali. 5 lye, which is connected to a space 86 above the plate. FIG. 10 shows a schematic representation of an 83. An oil outlet pipe 87 goes through the side view of an arrangement of the plates within the cover 84 into the oil collecting space 82. From the space of the vessel, FIG. 11 shows a top view of a distribution pipes 88 for the alkali lye from plate with fewer openings or holes than in the downward direction the oil sump and holes 77 F i g. 10 is shown * and F i g. 12 shows a section io of the topmost of the plates 73 from. Below the line AA in FIG. 11. Lowermost of the plates 73 is a collecting space 89 for

In Fig. 10, the used alkali with an outlet tube 72 a series of round or circular 90 for the used alkali is provided within a cylindrical Ge. Oil-in-plates 73 of the same design are shown, which outlet pipes 91 enter the upper part of this space through spacers 74, which emerge through holes 75 a 15 in such positions that rods or rods 75 not directly in the plates go on - under any of the holes in this plate ■ screwed and on the walls of the vessel means.

Rubber rings 76 are tightly connected. Every operation is an alkaline solution continuously

Plate is fed with a number of circular holes through the inlet tube 85, which provide the space 77 and 78, the holes 77 larger than ao 86 filling and through the tubes 88 are down and then the holes 78 and the distance d (cf. Fig. 11) over the surface of the second of the plates 73, through between each hole of a particular size and the tubes or lugs 80 over the surface of the next hole of the same size is constant. next plate and through the tubes 80 of the same. The holes are arranged so that when two etc., as indicated by the downward pointing arrows, plates are placed one on top of the other so that 35 points to the collecting space 89 for the used speaking holes match, while turning alkali and flows through the outlet pipe 90. While one plate is at 120 ° with respect to the other, the oil flows through the inlet pipes 91 in one direction towards the small holes in the upper plate along the underside of the lowermost plates with the large holes in the lower plate over and through the annular ones Match spaces 81 upwards, but not a small hole in the lower 30 and then match a hole in the top plate along the lower surface of the plate, next plate and through the annular spaces. The number of plates may range from 20 to 200 depending on the number of plates upwards, etc., as indicated by the arrows directed upwards from the process conditions in the range of 20 to the oil sump. 82, from which it then flows out through the oil outlet 87

A suitable arrangement of holes can be drawn.

can be obtained by an execution wherein a while running the oil in countercurrent

Lattice of equilateral triangles with a side d to the flow of the alkali, the neutralization is applied to a plate, with one of free acid in the oil continuous with a line XY of the lattice through the center O da- effectiveness of the renewal instead which goes from, where the closest vertex P has a 40 surface contact between the phases which is kon-spacing of d / 3 from this center. Each timely as a result of the passage of the oil through the apex of the lattice called the center point of the annular spaces takes place, depends on a small hole. This grid is then around The invention is described below with reference to

Rotated 60 ° C above the center of the plate. Then an example is explained in more detail, each vertex draws the center of a 45

big hole. This embodiment can be used in example 1

a sufficiently large continuation against the

Edge of the plate an excess of one hole. The device shown in FIG. 7 was used.

size over the other as shown in Fig. 11 at. Each guide plate was of which there are 16 large and 18 small holes 50 3.5 m and a width of 10 cm and down, produce. This should be avoided and with jumping flanges of 1 cm height, the production of the diagrammatically shown in FIG. 11. Two series of tests were carried out, namely

The two small holes were placed on the plate, and one was borrowed in which the lines (and their guides are furthest from the center, movement plates) at 7 ° to the horizontal and one, calmly. 55 at which these were inclined by 10 °.

The plates are around the edges of each hole The oil to be treated consisted of non-raffi-

flanged to match the hole in the nated coconut oil containing 3.9% In the middle to form a funnel or drain. (The free fatty acids.

The creation of flanges is useful when the alkaline solution consisted of a 0.4 n-

punching the hole carried out in the plate.) The 60 sodium hydroxide solution in water. The temperature Lugs or drains 79 (spouts) of the large holes 77 in the lines were kept at about 90 ° C, occur upward while the noses or drains. The results are in Table I below

of the small holes 78 (which passages are listed for the. In this table the specified Downward flow of the alkali lye through the device - throughputs of oil and alkaline solution in liters each the guide plate protrudes downwards into the large holes 77 65 centimeters wide per hour, with annular spaces 81 for being pressed on. The percentages of free fatty acids Downward flow of the oil left free through the device (f. f. a.) and of soap are to the weight of the consumed. holding refined oil.

Table I.

Tilt
the plate

7 °

7 °

7 °

10 °

Throughput

Oil / alkali

1 / cm / hour

1.0 / 0.6
2.0 / 1.2
2.0 / 1.2
2.0 / 1.2

Refined oil

»/ O f. F. A.

0.12
0.17
0.14
0.16

° / o soap

0.02
0.02
0.02
0.02

Example 2

The procedure described in Example 1 was followed except that a large part of the alkali solution emerging from the upper line after the addition of a small proportion of fresh alkali was recycled. This was done by taking the stream of Alkali solution increased to 8 times its value in Example 1, the circulated alkaline solution Solution with one seventh its volume of fresh alkaline solution on the inlet side of the device offset and continuous an equal volume of alkaline solution on the outlet side withdrew.

The results obtained are shown in Table II below, in which column 2 shows the throughput of fresh alkali lye.

Table II

Tilt
the plate Throughput
Oil / alkali
1 / cm / hour Refined oil
o / of.fa I% soap 0.02
0.02
0.03 7 °
7 °
10 ° 1.0 / 0.6
2.0 / 1.2
2.0 / 1.2 0.11
0.14
0.13

Example 3

It was shown in FIG. 1 device shown with the modification that the baffle plates 4 used in Fig. 5 had the training shown, the guide plate 4 cm wide and 180 cm long and to the horizontal Was inclined at an angle of 7 °, with the baffles (33 in number) were horizontal and the guide plate was mounted in a glass tube with an inner diameter of 5 cm. the The oil solution and the alkaline solution were flowing through the pipe in the same direction at speeds from 2 and 1.21 / cm / h guided. The oil jets had an upward path of about 1.5 cm in the transition from one baffle to the next.

The treated oil consisted of coconut oil with a free acid content of 3.8%. The alkaline The solution was a 0.4N sodium hydroxide solution. The free fatty acid content of the refined Product was 0.2-0.3%.

Example 4

The refined oil obtained in Example 3 was subjected to further refining treatment which included the

ίο was the same as that described in example 3, subject, the free fatty acid content being reduced to about 0.07%.

In Examples 3 and 4, the baffle plates described can be replaced by baffle plates of the type shown in FIGS. 4th or 6 shown training can be replaced. With flat or level baffle plates, as in FIG. 3 shown the reduction in the free fatty acid content was lower, with a great tendency towards Emulsification was present, which resulted in a larger oil

ao loss leads.

The effectiveness in these examples could be increased by adding the round Pipe through a conduit of rectangular cross-section, in which the guide plate in tight Adjacent to the top wall is attached to dead or unused space above the slab to avoid being replaced.

Example 5

The device was composed of two units arranged in series. The first was from a line of rectangular cross-section, a width of 10 cm and a length of 340 cm and was parallel with a simple rectangular flanged guide plate aligned with the axis of the duct, which adjoined the top wall, the plate and the pipe or conduit was inclined 10 ° to the horizontal.

The second unit consisted of a 22-plate zigzag tower (as in F i g. 8), each plate near its upper end ten holes (59, 60) with one Each had a diameter of 0.2 cm and the plates had a slope of 9 to 10 °.

These units were connected in such a way that the oil first went up through the pipe, then up were passed through the tower, it being in turn passed through the lower surface of each plate and passed from plate to plate through holes 59 and 60), while the alkaline solution (under the oil layer) first went up through the pipe and then up through the tower.

The product had a free fatty acid content of 0.02 to 0.07%. The "refinement factor" determined as

Weight of Crude Oil - Weight of Refined Oil

Weight of free fatty acid in crude oil - Weight of free fatty acid in refined oil

was only 1.3. The percentage of soap in the refined oil was only 0.02 to 0.04.

Example 6

The apparatus as described in Example 5 was used with the modification that the Line and its guide plates were 200 cm long and 5 cm wide and the tower with 34 zigzag arranged plates was provided, the slope of the plates was 3 to 4 ° and short tubes Corresponding to each hole in the plates were provided to the oil flows through the alkaline solution to carry from one plate to the next. The distance between the top of these tubes and the bottom surface of the next plate was about 0.4 cm.

The treated oil and the alkali solution were those given in Example 5 and the direction of the The flow of oil and the alkaline solution was as given in this example. The extent of the Flow was 11 to 141 per hour for the oil and 141 per hour for the alkaline solution.

The refined oil had a free fatty acid content of 0.06-0.09%, the soap content of the refined oil was 0.01% and the refining factor was 1.2 to 1.3.

Example 9

The procedure of Example 7 was repeated with the modification that the alkaline solution 5 was 0.8 N sodium hydroxide solution. The product showed a free fatty acid content of 0.09 to 0.13%, a sweet soap content of 0.01%, the Refining factor was 1.19.

Example 7 The refining was carried out in a tower

Example 10

The procedure was carried out in the manner described in Example 7 using an alkaline Solution of 0.2 N sodium hydroxide solution carried out. The product consisted of a mass with

guided, which with guide plates in zigzag 15 a content of free fatty acid of 0.18% and arrangement, as described with reference to FIG. 9, a soap content of less than Ο, ΟΙ * / »,
The product was collected in a vessel in

17 cm long and 17 cm wide from which an alkaline solution of O, 2N sodium-5 cm was present. Each plate had a near hydroxyd continuous at an extent of 41 to its upper end a hole of 0.8 cm through- up per hour. The jar was equipped with a knife, and each hole was fitted with a short tube single-blade stirrer fitted to rotate the alkaline solution down at 100 rpm. The oil layer on the underlying plate to mix oil and alkali was in a centric tray. The upwardly protruding flanges 70 and hollow bowl type zen-71 at one end of each plate had been trifuged to a height of about 30,000 rpm. That of 0.4 cm. Housing of the centrifuge was ER- to about 90 ⁰ C

The treated oil was coconut oil with a heater. The diameter of the separation or separation of free fatty acids of 4.4%. The alkaline manure cylinder in the centrifuge was 40 mm. The solution consisted of 0.4N sodium hydroxide solution. Content of free fatty acids in the thus treated oil was in the tower immediately below 30 oil was 0.01%. The refinement factor was determined on the bottom plate at a level of 151 each at 1.14.
Hour introduced and rose, guided by the lower “. · 1 -j 1

Surface of each plate, again on the example 11 above

End of each plate upwards, with it upwards. The refining was in a tower which

through an opening or gap (68 or 69) at 35 with a zigzag guide of the next plate poured, plates as with reference to FIG. 9 has been carried out,

The alkaline solution was run into the room above it, being in the tower half of the top plate at the top of it
an amount of 151 per hour and

flowed down in contact with the upper surface of 4 ° 0.9 cm in diameter near its upper end in front of each plate and passed again from one hand; each hole was provided with a short plate to the one below through the tubes 66 pipe, through which the solution down or 67th through the oil layer on the plate below

The product had a free fat content that was worn. The slope of the plates was 5 °. acid from 0.08 to 0.14%, the soap content 45. The upwardly protruding flanges 70 and 71 am 0.01% and the refining factor was 1.2. The end of each plate had a height of 0.6 cm and

ended 0.17 cm below the next upper plate.

Example 8 The treated oil consisted of lower sebum

Quality with different levels of free fat - The procedure was as in Example 7 under 5 ° acid. The oil was both in cocurrent as well

40 plates each with a length of 17 cm and a width of 10 cm and two holes of each

Turning a 0.2 N sodium hydroxide solution carried out as an alkaline solution. Owned the product a free fatty acid content of 0.14 to 0.17%, a soap content of 0.01% and the refining factor was 1.12.

in countercurrent with the alkaline solution using. different alkali concentrations and different throughputs.

The results are shown in Table III below.

Table ΠΙ

attempt % free
fatty acid Alkali
concentration oil flow rate
ία m ³ / hour / m width % ff, a.
refined oil Alkali Oil Stream 1
2
3
4th
5 3.66
3.66
3.66
5.16
5.16 0.1 normal
0.2 normal
0.2 normal
0.1 normal
0.1 normal 0.20
0.30
0.30
0.20
0.20 0.24
0.28
0.36
0.27
0.57 Countercurrent
Countercurrent
Direct current
Direct current
Countercurrent

Example 12

Low quality sebum has undergone a refining or refining treatment in one subjected to two series-arranged units existing device.

The first unit consisted of a pipe with a rectangular cross-section and a width of 10 cm and a length of 200 cm, which is fitted with a simple flanged rectangular guide plate in parallel alignment with the axis of the conduit and adjacent to its top wall was with the plate and the conduit inclined at 10 ° to the horizontal.

The second unit consisted of a tower of the type described in Example 11. The oil initially rose up through the pipe and then, after overflowing over a dam, it became into the Pumped tower. Fresh alkali flowed either cocurrently or countercurrently in the tower to the oil.

ίο The results obtained are in the following Table IV listed.

»/Of.f.a. Alkali concentration Table IV »/Of.fa
refined oil Flow way attempt 3.66
5.16
5.56
5.47
5.47 0.1 normal
0.1 normal
0.2 normal
0.1 normal
0.1 normal Oil flow
in m ³ / hour / m width 0.14
0.28
0.41
0.28
0.20 Direct current
Direct current
Countercurrent
Direct current
Countercurrent 1
2
3
4th
5 0.20
0.20
0.30
0.20
0.20

Example 13

The procedure of Example 11 was carried out using low quality sebum with a Free fatty acid content of 5.02%. The product had a free content Fatty acids of 0.40% and a soap content of 0.01%.

The product was collected in a vessel equipped with a stirrer and concentrated Alkali solution of 4N was added. After stirring for 3 minutes, hot water was in a added in such an amount that the theoretical concentration of the alkali was determined to be 0.2 normal. The mixture was heated and held at 90 ° C., after which, after stirring for 10 minutes, the soap was decanted off became.

The free fatty acid content in the obtained oil product was 0.02%.

Example 14

In a device of the type shown in FIGS Coconut oil has been refined in the embodiment shown.

The cylindrical vessel 72 was 500 mm in diameter and 390 mm in height. Within the vessel 22 horizontal plates 73 were provided, which were supported by seven rods 75, the attached to the bottom of the jar were held in place. The panels were at a distance of 10 mm from each other by means of spacers 74 held and attached. In every record there were 16 openings 77 with a diameter of 32 mm, each one pointing upwards Flanges, which formed a funnel or a nose 79, had 16 and openings 78 with a diameter of 11.5 mm each with a downwardly directed flange, which has a nose or a funnel 80 made. The holes were arranged according to the pattern shown in FIG. During the Attachment, each plate was rotated 120 ° with respect to the underlying plate so that the Tubes or noses from the small openings in one plate into the large openings in the plate below protruded. This created a path through the annular space 81 between the noses or tubes the small openings and the edges of the large openings into which they protruded. the The length of the path could be changed by changing the perpendicular distance between the plates the spacers can be varied. The top and bottom plates were with 16 small inlet tubes 88 for the alkali and 16 small inlet pipes 91 for the oil. In the cover 84 of the Apparatus was provided with the main inlet line 85 for the caustic solution and the oil outlet 87, and The outlet 90 for the used alkali was provided in the base plate (without reference number).

The vessel was first charged with the alkali, which filled the space between the plates. Oil was then introduced at the bottom, which passed up along the underside of the panels the annular space 81 rose into the oil collecting space 82. The alkali was continuously poured into the System through inlet 85 and oil through inlets 91 supplied, with refined oil through outlet 87 and the spent caustic through the Outlet 90 were removed.

Raw coconut oil with a free fatty acid content of 4.67% and a moisture content of 0.17% was refined by treatment in the device with a 0.1 N alkali solution. The speed of the oil was 1001 per hour and about 109.5 kg of oil was treated. The content of free fatty acids of the refined oil was 0.29 and the soap content was 0.115. The refinement factor was 1.02.

The invention has been described with particular reference to the refining of coconut oil. A variety of other glyceride oils can be refined in the same manner, including

z. B. palm oil, palm kernel oil, peanut oil, cottonseed oil, soybean oil, rapeseed oil, sunflower oil and safflower oil, as well as animal oils and oils from marine animals, such as lard or pork fat, tallow, Whale oil and fish oils, which are both hardened and can be uncured. As can be seen, the process must be carried out at a temperature in which the treated oil is sufficiently mobile to flow easily through the device. Tem-

909 503/1549

Temperatures from 70 or 80 ° C to over 90 ° C are generally advantageous, and in particular were get good results even at higher temperatures, for example at 95 to 100 ° C.

The invention comprises suitable apparatus for carrying out the method according to the invention. Such a device may include a device which allows a flow of a current in a alkaline solution caused along a predetermined path, on which any tendency to the Horizontal is small, an inlet device for the solution at one end of this path, an outlet device for this solution at the other end of this path, an inlet device for the introduction of the oil above the level of this solution at one end of this path which is no higher than the other end is, and guide means for guiding the oil layer along in succession from each of a series of paths in which each inclination to the horizontal is upward with a little Angle is directed thereto, include, wherein the guide device is formed and arranged is that between successive paths of this series the contact of the oil with any layer an aqueous soap solution which has been formed without substantially mixing the oil with the alkaline solution or the soap solution is interrupted.

In general terms, the device according to the invention comprises a system of lines for Carrying or carrying oil and aqueous alkali, an inlet for the aqueous alkali at one end of the system and an outlet therefor at the other end, an oil inlet at one end of the system and an outlet therefor at the other end, within the system a plurality of guide members, each having a guide surface over a series of spaced apart Staggering, which extends along this, have, said staggering parts of a diverted path for oil and aqueous alkali, each going from the corresponding inlet to the corresponding Outlet flow, the oil along most of the way on the surface of the aqueous Layer flows and any inclination of the staffein to the horizontal upwards in the direction of the oil flow is at an angle not greater than about 10 °, and means between the front end in that direction of each such relay and the rear end of the following Relay provided to interrupt the boundary or intermediate surface between the aqueous and the oil layer or attached, whereby a separate implementation of oil and alkali solution in contiguous Flowing from this season to the next season is effected.

As indicated above with reference to the drawing, one suitable arrangement includes an inclined conduit in which a guide plate for the oil layer with attached baffle 6a or baffles attached to create the separate paths in the order listed, wherein Holes or tubes near the end or teeth at the end of the baffles or baffles for breaking or dividing the oil layer and alkaline solution in separate streams are provided, the oil layer from one path to the next steeply upwards in the form of continuous streams flows so that substantial mixing with the alkaline solution or the soap solution is avoided will.

According to a further embodiment, the device according to the invention comprises with reference to FIG F i g. 7 a plurality of separate inclined pipes each equipped with a guide plate are, with the oil layer at the top of a line from the alkaline solution and the Soap layer separated and through a separate or special pipe to the lower end of the subsequent Line is led.

With reference to Figures 8 and 9, the apparatus comprises according to the invention a zigzag arrangement of plates with a substantially vertical gap between the top of one and the bottom of the other subsequent Plate, with suitable means for effecting the desired separation of oil from the aqueous Media without significant mixing are provided. For example, such means as in Fig. 8 shows holes (or tubes) near the upper ends of the plates for the passage of the oil in separate vertical streams passing through the aqueous medium flow without mixing and leave a gap between the downwardly protruding end flange at the top of each plate to collect the stream of aqueous medium. on the other hand can, as in FIG. 9, tubes may be provided to stream the alkaline solution into which go through the oil layer without touching it, breaking or dividing, the oil layer straight up through a gap between the upwardly extending end flange flows at the top of the plate and the housing in contact with the next plate.

The in the F i g. 10 to 12 has the device shown compared to the foregoing the advantage that they result in an economically and technically advantageous floor plan.

Claims (14)

Patent claims: 1. Process for alkali refining of glyceride oils, in which these in the form of thin layers with an aqueous alkaline solution treated with the oil arranged along the bottom of in the alkaline solution solid surfaces flows, characterized in that both the oil and the aqueous alkaline solution in the same or in the opposite direction continuously through a plurality of treatment zones leads, which are limited at the top by the fixed surfaces and laterally by guide surfaces and the transition of the oil from each zone to the next higher with such a sharp change of direction occurs that the side film formed at the interface oil-alkaline solution in each zone tears off and is distributed in the alkali solution, and the neutral oil obtained and the soap-containing one aqueous alkali solution continuously discharges separately. 2. The method according to claim 1, characterized in that the oil and the aqueous Alkali solution leads in a tortuous path, which is a series of spaced Comprises staggering of the solid surfaces, the Interface between the aqueous layer and the oil layer at the end of each zone in direction the oil flow is interrupted and the oil and the alkaline solution in contiguous Streams from each zone to be transferred to the next. 3. The method according to claim 1 or 2, characterized in that the oil layer at the end of each zone is forced to change its direction of flow and to travel a vertical path, which is at most equal to the distance over which the oil meets the guide surface of the relevant Zone was in contact. 4. The method according to any one of claims 1 to 3, characterized in that the oil layer and the aqueous alkali solution can be transferred separately from one zone to the next. 5. The method according to any one of claims 1 to 4, characterized in that the width of the Oil layer at the end of each zone reduced in the direction of the ao oil flow. 6. The method according to any one of claims 1 to 5, characterized in that at the beginning of the Refining adds a small amount of a wetting agent and / or salt. 7. Device for performing the method according to one of claims 1 to 6, with a Refining tank in which guide plates for the oil are arranged and the one at the lower end is provided with a feed device for the oil to be refined, characterized by a plurality of staggered guide plates which are arranged at a vertical distance from one another and which are arranged separately from one another, which are provided with lateral, downwardly directed limiting flanges, and by devices for continuous supply and discharge of both oil and alkali solution. 8. Apparatus according to claim 7, characterized in that the guide plates (4) in Direction converge towards their free end or their width is reduced by recesses (20) and / or are provided with openings (24) or the flow-restricting parts (19, 22). 9. Apparatus according to claim 7, characterized in that guide plates (55, 56) are opposite are arranged obliquely in a housing (54), downwardly directed at their upper end Have flanges (57 and 58) and near the upper end openings (59, 60) for Dividing the oil film into a number of separate, upwardly flowing streams, wherein between the flanges (57 and 58) of the guide plates and the wall of the container (54) Openings (61, 62) provided for the passage of the alkaline solution without disturbing the oil flow are. 10. The device according to claim 9, characterized in that instead of the openings (59, 60) upwardly extending pipes are provided for the flow of oil. 11. The device according to claim 7, characterized in that that guide plates (64, 65) are arranged at an opposite angle in a housing (63) each plate is equipped at the top with tubes (66, 67) extending downward and allow separate passage of the alkaline solution, openings (68, 69) between the wall of the container (63) and the guide plates (64, 65) for passing through of the oil are provided. 12. The apparatus according to claim 11, characterized in that at the upper end of each guide plate a flange (70, 71) is provided which extends upwards to below the lower end of the next higher guide plate extends. 13. The apparatus according to claim 7, characterized in that each guide plate (73) one Number of large and small openings (77, 78), of which the small openings (78) each with a downwardly protruding tube (80) and the large openings (77) each are provided with an upwardly projecting tube (79), the tube (80) of each small Opening (78) opens into a large opening (77) in the plate below an annular space (81) for the upward passage of the oil, the openings (77, 78) are arranged offset from one another and the device (85) for continuous Supply of the alkaline solution is arranged above the top plate (73). 14. Apparatus according to claim 13, characterized in that a plurality of circular matching plates (73) in a cylindrical container (72) one above the other is arranged that the centers of each small opening (78) in the higher plate with those each large opening (77) in the underlying plate coincide. For this purpose 2 sheets of drawings