The present invention is concerned with a continuously operating separating apparatus for the separation of mixtures of light and heavy liquid components which apparatus comprises
a mixing portion, which is located in the middle portion of said apparatus and which comprises a mixing vessel and a cylinder placed in the middle of said mixing vessel, whereat said mixing vessel and said cylinder constitute the mixing zone, and
a separating portion, which is located in the upper portion of said apparatus and which comprises two or more cones placed one inside the other, whereat said cones constitute the separating zone, and
a circulating pump, which is connected by means of two or more conduits tangentially to said mixing vessel, and
a bottom portion, and
a feed conduit, which is connected to the upper portion of said mixing vessel tangentially, and
discharge members located in the upper portion of said apparatus, said discharge members comprising an overflow member and discharge outlets, through which the light liquid fraction is discharged, and
a substantially vertical discharge member placed in the middle of said apparatus, through which member the heavy liquid fraction is discharged.
The separating apparatus may also be provided with a discharge member extending to the bottom of said apparatus, the solid matter sinking to the bottom part being discharged through said discharge member.
The invention is also concerned with a method for the separation of mixtures comprising dispersions of liquids of different densities wherein the mixture is fed tangentially into the mixing zone of the separating apparatus, in which zone the mixture is circulated tangentially by means of a pump between the cylinder placed in the middle of said apparatus and the mantle of the mixing vessel, whereat the lighter liquid phase rises into the separation zone located in the upper portion of said separating apparatus and comprising two or more cones placed one inside the other, and is discharged as overflow from the upper portion of said apparatus, whereas the heavier liquid phase is discharged through the cylinder and the discharge member placed in the middle of the cylinder.
The diameter of the cylinder 5 is 1/2 to 1/5 of the diameter of the mixing vessel 4, preferably 1/3 to 1/5 of the diameter of said vessel.
This invention was conceived and perfected in connection with research involving the separation of tall oil from tall oil skimmings. It will be described in reference to said separation, with the understanding that it is capable of broader application, being applicable to the separation of any mixture comprising liquid components having different densities.
More particularly, the invention is concerned with a method for the separation of tall oil and similar products from an acid tall oil soap mixture which contains 20 to 55% of tall oil, 45 to 80% of mother liquid, whose pH is 2 to 3.5, and less than 10% of lignin, as well as varying quantities of gypsum, whereby said mixture is fed at a rate of 1,000 to 10,000 kg/hour tangentially into the mixing zone of the separating apparatus, in which the mixture is circulated tangentially by means of a pump between the cylinder placed in the middle of the apparatus and the mantle of the mixing vessel at a rate of 10 to 100 m.sup.3 per hour, whereat the lignin is dispersed in the mother liquid, and the tall oil, being of lower weight, rises into the separating zone located in the upper portion of said apparatus and consisting of conical discs placed one inside the other, and is discharged as overflow from the top portion of said apparatus, whereas the mother liquid and the lignin dispersed in same are discharged through the cylinder and the discharge pipe placed in the middle of the cylinder.
From the U.S. Pat. No. 2,838,481, a method is known for the separation of tall oil and similar products by treating a dilute tall oil soap solution obtained by adding water and acid to tall oil skimmings in a high-performance agitator and by recovering the hydrolyzed products. In the recovery, a centrifuge is used. The apparatus also includes a continuously vibrating strainer, whose function is, among other things, to separate any cellulose fibres interfering with the centrifuging operation.
Another common method for the recovery of a product of hydrolysis is decanting. In such a case, the apparatus is, however, very large, the cleaning is laborious, and, moreover, the interval between cleanings is short, and the separation takes place slowly.
Now, a novel separating apparatus has been invented, by means of which mixtures of light and heavy liquid components can be separated, such as mixtures containing tall oil and similar products, can be separated efficiently.
By means of the apparatus in accordance with the invention, it is possible to treat all types of dispersions of oil and water, such as oil-containing waters, in particular oil-containing sewage waters, and also oily and aqueous sludges, such as sewage waters that contain sludge.
Said new apparatus has the following advantages as compared with the apparatus including a centrifuge, described in the U.S. Pat. No. 2,838,481:
the new apparatus is simpler and it has no moving parts,
when the new apparatus is used, the consumption of energy and the forces of friction are low, and
the cleaning of the new apparatus is easy, and, moreover, the intervals between cleanings are long.
In the following, the invention will be described in more detail with the aid of the exemplifying embodiments, and the drawings, which are shown for purpose of illustration only.
FIGS. 1 and 4 are schematical views of a separating apparatus in accordance with the invention.
FIG. 2 shows a separating apparatus in accordance with the invention.
FIG. 3 is a vertical sectional view of a separating apparatus in accordance with the invention.
The separating apparatus in accordance with the invention comprises a mixing portion 3, which is located in the middle portion of said apparatus, and a separating portion, which is located in the upper portion of said apparatus, and a bottom portion 13, as well as means for feeding the mixture to be separated and means for discharging the separated products.
Said mixing portion 3, which is located in the middle portion of said apparatus comprises a mixing vessel 4, a vertical cylinder 5 located in the middle portion of said mixing vessel, a feed pipe 19 for the mixture to be separated, connected tangentially to said upper portion of said mixing vessel, and a circulating pump 2, which is connected tangentially to said middle portion of said mixing vessel by means of two or more circulating pipes 17, 18.
Said separating portion, which is located in the upper portion of said apparatus, comprises 2 to 10 cones 7 placed one inside the other, the distances between said discs being 50 to 200 mm and the angle of said cones being less than 90.degree., preferably about 60.degree., discharge members for the light component of the mixture, i.e. an overflow member 8 and collecting pipes 25 and discharge pipes 26, and a vent pipe 21.
The bottom portion 13 is preferably conical in shape and it is provided with a sediment discharge pipe 16.
The discharge member for the discharge of the heavy component of the mixture is located in the middle of said apparatus, partly inside the cylinder 5, said discharge member comprising a discharge pipe 10, a telescopic pipe 11 located in its upper portion, and an adjusting member 12 for said telescopic pipe. The mantle 4 of the mixing vessel is provided with one or several view glasses 22, and the cover of the separating portion is provided with several, preferably four, inspection holes 28.
According to the method in accordance with the invention, the mixture to be separated is passed into the mixing vessel located in the middle portion of the apparatus, into the mixing zone formed by the mantle 4 of the mixing vessel and of the cylinder 5 located in the middle of the mixing part, wherein the mixture is circulated intensively by means of the pump 2, as shown in (FIG. 1, arrow 3). Thereat, the light components of the mixture move upwards (FIG. 1, arrow 6), and the heavy components move downwards (FIG. 1, arrow 9). By adjusting the telescope pipe 11 by means of the adjusting member 12, it is possible to keep the interface between the phases at an appropriate level, which is 0 to 50 cm above the upper edge of the mixing portion. In the separating portion, the drops of the heavy phase are separated from the light phase very efficiently and flow down along the cones 7. The separated light phase is discharged as overflow via the discharge members 8, 25 and 26. The heavy phase rises into the funnel 5 and is discharged through the pipe 10.
Any gases and water vapour are discharged through the vent 21 located in the top portion of the apparatus.
Any heavy materials sinking to the bottom of the apparatus, such as gypsum, are discharged through a pipe 16 extending to the bottom of the apparatus.
The removal of the heavy phase so that the interface between the light fraction and the heavy fraction remains at the level of 0 to 0.5 m above the upper edge of the mixing vessel is performed by means of an adjustable telescopic pipe 11 or by means of a control valve 30, 33 and 34 and by means of two or more limit switches 31 and 32 or by means of any other detector of the interface (FIG. 4).
The capacity of the separator apparatus is very high, the fed rate is between 1000 and 10,000 kg/hour, preferably between 1000 and 7,000 kg/hour, the volume of the mixing portion being between 1 and 5 m.sup.3.
While one specific embodiment of the invention has been described in detail above, it is to be understood that various modifications may be made from the specific details described without departing from the spirit and scope of the invention.
The following examples illustrate the method in accordance with the invention.
Example 1
Into a separating device having a volume of about 1.7 m.sup.3 (mixing portion of about 0.6 m.sup.3, separation portion of about 1.0 m.sup.3 and bottom cone about 0.1 m.sup.3), was passed a tall oil soap mixture obtained by mixing together 1300 kg/h of tall oil skimmings separated from black liquor and 560 kg/h of 30-% sulfuric acid the mixture containing 45% of tall oil (density 960 kg/m.sup.3), 45% of mother liquid (density 1106 kg/m.sup.3, pH 3.2) and 8% of lignin (density 1060 kg/m.sup.3) as well as 2% of gypsum, at a rate of 1860 kg per hour, at 90.degree. C. The mixture was passed tangentially through the pipe 19 into the mixing zone 3 of the device, wherein, by means of a circulating pump 2 tangentially connected to the mixing vessel, a rotary movement was imparted to the mixture in the space defined by the mantle 4 of said vessel and the cylinder 5 located in the center of said vessel. The intensity of the circulation was 23 m.sup.3 per hour. From the top of the device the tall oil was discharged as overflow 8, 25, 26. The mother liquid and the lignin dispersed in same flowed into the discharge pipe 10 and were discharged through the bottom part of the device. The telescopic pipe 11 located in the upper portion of the discharge pipe 10 was adjusted so that the interface between the tall oil and the mother liquid was approximately at the level of the upper edge of the mixing portion.
The analysis of the separated tall oil was:
Tall oil: 97% by volume
Lignin: 3% by volume
Mother liquid: --
Gypsum: --
The analysis of the separated mother liquid was:
Tall oil: 2% by volume
Lignin: 1% by volume
Mother liquid: 96% by volume
Gypsum: 1% by volume
Example 2
Into the separating device, described in Example 1, was passed a tall oil soap mixture obtained by mixing together 820 kg/h of tall oil skimmings separated from black liquor and 610 kg/h of spent acid derived from the preparation of chlorine dioxide (composition: sodium sulfate 360 g/l, sulfuric acid (100%) 456 g/l, and sodium chlorate about 3 g/l) and which mixture contained 55% of tall oil (density 960 kg/m.sup.3), 40% of mother liquid (density 1106 kg/m.sup.3, pH 2.2) and 5% lignin (density 1060 kg/m.sup.3) as well as <1% of gypsum, at a rate of 1430 kg per hour, at 90.degree. C. The mixture was passed tangentially into the mixing zone 3 of the device, wherein the intensity of the circulation was 19.5 m.sup.3 per hour. From the top of the device the tall oil was discharged as overflow 8. The mother liquid and the lignin dispersed in same flowed into the discharge pipe 10 and were discharged from the bottom portion of the device. The telescopic pipe 11 located in the upper portion of the discharge pipe 10 was adjusted so that the boundary surface between the tall oil and the mother liquid was 0.1 m above the upper edge of the mixing portion.
The analysis of the separated tall oil was:
Tall oil: 98% by volume
Lignin: 2% by volume
Mother liquid: --
Gypsum: --
The analysis of the separated mother liquid was:
Tall oil: 2% by volume
Lignin: 4% by volume
Mother liquid: 94% by volume
Gypsum: --
Example 3
Into the separating device, described in Example 1, was passed a tall oil soap mixture obtained by mixing together 1715 kg/h of tall oil skimmings separated from black liquor and 415 kg/h of spent acid derived from the preparation of chlorine dioxide (composition: sodium sulfate 360 g/l, sulfuric acid (100%) 456 g/l, and sodium chlorate about 3 g/l) and which mixture contained 25% of tall oil (density 960 kg/m.sup.3), 70% of mother liquid (density 1118 kg/m.sup.3, pH 2.2) and 4% of lignin (density 1060 kg/m.sup.3) as well as 1% gypsum, at a rate of 2130 kg per hour, at 94.degree. C. The mixture was passed tangentially into the mixing zone 3 of the device, wherein the intensity of the circulation was 24 m.sup.3 per hour. From the top of the device the tall oil was discharged as overflow 8. The mother liquid and the lignin dispersed in same flowed into the discharge pipe 10 and were discharged from the bottom part of the device. The telescopic part 11 located in the upper portion of the discharge pipe 10 was adjusted so that the interface between the tall oil and the mother liquid was 0.3 m above the upper edge of the mixing portion.
The analysis of the separated tall oil was:
Tall oil: 95% by volume
Lignin: 3% by volume
Mother liquid: 1% by volume
Gypsum: 1% by volume
The analysis of the separated mother liquid was:
Tall oil: 2% by volume
Lignin: 2% by volume
Mother liquid: 94% by volume
Gypsum: 2% by volume
Example 4
Into a separating device having a volume of about 1.7 m.sup.3 (mixing portion of about 0.6 m.sup.3, separation portion of about 1.0 m.sup.3 and bottom cone of about 0.1 m.sup.3) was passed a mixture containing 32% of tall oil (density 950 kg/m.sup.3), 62% of mother liquid (density 1100 kg/m.sup.3, pH 3.0) and 6% of lignin (density 1060 kg/m.sup.3) at a rate of 600 kg/h at 80.degree. C. The mixture was passed tangentially through a pipe 19 into the mixing zone 3 of the device wherein, by means of a disposed recirculation pump 2, tangentially connected to the mixing vessel a rotary movement was imparted to the mixture in the space defined by the mantle 4 of said vessel and the cylinder 5 located in the center of said vessel. The rate of circulation was 16 m.sup.3 per hour. From the top of the device the tall oil was discharged as overflow 8, 25, 26.
The mother liquid and the lignin dispersed therein flowed into a discharge pipe 10 and were discharged through the bottom of the device. The telescopic pipe 11 located in the upper portion of the discharge pipe 10 was adjusted so that the interface between the tall oil and the mother liquid was approximately at the level of the upper edge of the mixing portion.
The analysis of the separated tall oil was:
Tall oil: 98% by volume
Lignin: 1% by volume
Mother liquid: 1% by volume
Gypsum: --
The analysis of the separated mother liquid was:
Tall oil: 2% by volume
Lignin: 2% by volume
Mother liquid: 96% by volume
Gypsum: 1% by volume
Example 5
Same separation device as in Example 4 was used, and same operations. The composition of the feed mixture was as follows:
30% by volume: tall oil (density 950 kg/m.sup.3)
63% by volume: mother liquid (density 1105 kg/m.sup.3, pH 3.0)
7% by volume: lignin (density 1060 kg/m.sup.3)
Feed rate: 1000 kg/h
Feed temperature: 87.degree. C.
Circulation rate: 17 m.sup.3 per hour
The analysis of the separated tall oil was:
Tall oil: 99% by volume
Lignin: 1% by volume
Mother liquid: --
Gypsum: --
The analysis of the separated mother liquid was:
Tall oil: 2.0% by volume
Lignin: 3.0% by volume
Mother liquid: 95.0% by volume
Gypsum: --
Example 6
Same separation device as in Example 4 was used, and same operations.
The composition of the feed mixture was as follows:
32% by volume: tall oil (density 950 kg/m.sup.3)
60% by volume: mother liquid (density 1110 kg/m.sup.3, pH 3.0)
8% by volume: lignin (density 1060 kg/m.sup.3)
Feed rate: 1530 kg/h
Feed temperature: 87.degree. C.
Circulation rate: 20 m.sup.3 per hour.
The analysis of the separated tall oil was:
Tall oil: 98% by volume
Lignin: 1% by volume
Mother liquid: 1% by volume Gypsum: --
The analysis of the separated liquid was:
Tall oil: 2% by volume
Lignin: 3% by volume
Mother liquid: 95% by volume
Gypsum: --
Example 7
Same separation device as in Example 4 was used, and same operations.
The composition of the feed mixture was as follows:
24% by volume: tall oil (density 950 kg/m.sup.3)
65% by volume: mother liquid (density 1095 kg/m.sup.3, pH 2.3)
11% by volume: lignin (density 1060 kg/m.sup.3)
Feed rate: 1570 kg/h
Feed temperature: 90.degree. C.
Circulation rate: 20 m.sup.3 per hour.
The analysis of the separated tall oil was:
Tall oil: 99% by volume
Lignin: 1% by volume
Mother liquid: --
Gypsum: --
The analysis of the separated mother liquid was:
Tall oil: 2% by volume
Lignin: 3% by volume
Mother liquid: 95% by volume
Gypsum: --
Example 8
Same separation device as in Example 4 was used, and same operations.
The composition of the feed mixture was as follows:
26% by volume: tall oil (density 950 kg/m.sup.3)
67% by volume: mother liquid (density 1095 kg/m.sup.3, pH 2.8)
6% by volume: lignin (density 1060 kg/m.sup.3)
Feed rate: 2200 kg/h
Feed temperature: 88.degree. C.
Circulation rate: 21 m.sup.3 per hour.
The analysis of the separated tall oil was:
Tall oil: 98% by volume
Lignin: 1% by volume
Mother liquid: 1% by volume
Gypsum: --
The analysis of the separated mother liquid was:
Tall oil: 4% by volume
Lignin: 2% by volume
Mother liquid: 94% by volume
Gypsum: --
Example 9
Into a separating device was passed a crude tall oil water mixture obtained by mixing 490 kg/h of crude tall oil and 110 kg/h of hot water as well as 0.4 kg/h of 100% sulfuric acid. The composition of the feed mixture was as follows:
84% by volume: tall oil (density 950 kg/m.sup.3)
8% by volume: washing water (density 980 kg/m.sup.3, pH 3.2)
8% by volume: lignin
Feed rate: 600 kg/h
Feed temperature: 86.degree. C.
The mixture was passed tangentially into the mixing zone 3 of the device wherein the rate of circulation was 20 m.sup.3 /h. From the top of the device the tall oil was discharged as overflow 8. The washing water and the lignin dispersed therein as well as other impurities flowed into a discharge pipe 10 and were discharged through the bottom of the device. The telescopic pipe 11 located in the upper portion of the discharge pipe 10 was adjusted so that the interface between the tall oil and the washing water was approximately at the level of the upper edge of the mixing portion. The analysis of the separated washed tall oil was:
Tall oil: 96% by volume
Lignin: 3% by volume
Washing water: 1% by volume
Gypsum: --
The analysis of the washing water used was:
Tall oil: --
Lignin: 2% by volume
Washing water: 98% by volume
Gypsum: --
The reduction in the ash content of the tall oil was 88%.
Example 10
Same separation device as in Example 9 was used, and same operations.
The crude tall oil water mixture was obtained by mixing 550 kg/h of crude tall oil and 110 kg/h of hot water as well as 0.4 kg/h of 100% sulfuric acid.
The composition of the feed mixture was as follows:
80% by volume: tall oil (density 950 kg/m.sup.3)
15% by volume: washing water (density 980 kg/m.sup.3, pH 2.3)
5% by volume: lignin
Feed rate: 650 kg/h
Feed temperature: 87.degree. C.
Circulation rate: 20 m.sup.3 per hour.
The analysis of the separated washed tall oil was:
Tall oil: 99% by volume
Lignin: 1% by volume
Washing water: --
Gypsum: --
The analysis of the separated washing water was:
Tall oil: 1% by volume
Lignin: --
Washing water: 98% by volume
Gypsum: 1% by volume
The reduction in the ash content of the tall oil was 87%.
Example 11
Same separation device as in Example 9 was used, and same operations.
The crude tall oil water mixture was obtained by mixing 630 kg/h of crude tall oil and 60 kg/h of hot water as well as 0.3 kg/h of 100% sulfuric acid.
The composition of the feed mixture was as follows:
95% by volume: tall oil (density 950 kg/m.sup.3)
4% by volume: washing water (density 980 kg/m.sup.3, pH 1.8)
1% by volume: lignin
Feed Rate: 690 kg/h
Feed temperature: 88.degree. C.
Circulation rate: 20 m.sup.3 per hour.
The analysis of the separated washed tall oil was:
Tall oil: 99% by volume
Lignin: 1% by volume
Washing water: --
Gypsum: --
The analysis of the separated washing water was:
Tall oil: 1% by volume
Lignin: 1% by volume
Washing water: 98% by volume
Gypsum: --
The reduction in the ash content of the tall oil was 91%.
Example 12
Same separation device as in Example 9 was used, and same operations.
The crude tall oil water mixture was obtained by mixing 780 kg/h of crude tall oil and 55 kg/h of hot water as well as 0.5 kg/h of 100% sulfuric acid.
The composition of the feed mixture was as follows:
93% by volume: tall oil (density 950 kg/m.sup.3)
4% by volume: washing water (density 980 kg/m.sup.3, pH 2.1)
2% by volume: lignin
1% by volume: gypsum
Feed rate: 835 kg/h
Feed temperature: 96.degree. C.
Circulation rate: 20 m.sup.3 per hour.
The analysis of the separated washed tall oil was:
Tall oil: 98% by volume
Lignin: 1% by volume
Washing water: 1% by volume
Gypsum: --
The analysis of the separated washing water was:
Tall oil: 2% by volume
Lignin: 1% by volume
Washing water: 96% by volume
Gypsum: 1% by volume
The reduction in the ash content of the tall oil was 86%.
Example 13
Same separation device as in Example 9 was used, and same operations.
The crude tall oil water mixture was obtained by mixing 1450 kg/h of crude tall oil and 44 kg/h of hot water as well as 0.8 kg/h of 100% sulfuric acid.
The composition of the feed mixture was as follows:
95% by volume tall oil (density 950 kg/m.sup.3)
3% by volume: washing water (density 980 kg/m.sup.3, pH 1.5)
2% by volume: lignin
Feed rate: 1494 kg/h
Feed temperature: 85.degree. C.
Circulation rate: 20 m.sup.3 per hour.
The analysis of the separated washed tall oil was:
Tall oil: 97% by volume
Lignin: 1% by volume
Washing water: 2% by volume
Gypsum: --
The analysis of the separated washing water was:
Tall oil: --
Lignin: 1% by volume
Washing water: 99% by volume
Gypsum: --
The reduction in the ash content of the tall oil was 89%.