JPH0525521B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention generally relates to the use of water to remove amines from oil-amine components produced in the process of decomposing oil-water emulsions or sludges. Regarding the method, the method uses an amine that has an inverse critical solution temperature with water. More specifically, the present invention teaches a method for removing substantially all amines from an oil-amine component, wherein the amine is present in the oil-amine component in amounts as low as 10% by weight or less. . The present invention also teaches a method of controlling the amount of water required for the separation.

BACKGROUND OF THE INVENTION A method for dewatering sludge by the use of amines or mixtures thereof having inverted critical solution temperatures with water is published in Emanuel, August 12, 1975, and assigned to the United States. Patent No.
No. 3,899,419.
Improvements to such methods are disclosed in U.S. Pat. No. 3,925,201 to Ames and U.S. Pat.
No. 4,056,466.

Furthermore, Ams et al. in U.S. Pat. No. 4,002,562 describe emulsions and solid substances containing oil and water;
A method of destroying sludge containing oil and bound and unbound water is taught. The method taught by Ams is applicable to a wide range of oil-water emulsions (including oil-in-water emulsions and water-in-oil emulsions) and is suitable for waste materials that are difficult to treat by known methods. It finds particular utility in the treatment of emulsions as AMUS U.S. Patent No.
According to the method taught in No. 4,002,562, an amine or amine mixture having an inverted critical solution temperature with water is added to an emulsion or sludge, and the temperature of the resulting mixture is brought below the inverted critical solution temperature. If solid materials are present, they can be physically separated from the remainder of the mixture by various separation methods known in the art, such as centrifugation or filtration. After separation of the solid materials, the remainder of the mixture is a more or less homogeneous mixture of water, oil and amine. When the temperature of the water-oil-amine mixture is raised above the inverted critical solution temperature of the amine, two components are produced. That is, a water component containing a small amount of amine and an oil-amine component containing a small amount of water.

U.S. Pat. No. 4,002,562 to Amus describes the known method,
For example, methods are provided for removing the amine from the oil-amine mixture by distilling the amine and leaving an oil behind and recycling the amine. However, recovery of amines from amine-oil mixtures by known methods has proven extremely difficult. Also, an unacceptable amount of amine will be left in the oil, especially if the oil is to be recycled for further use.

When practicing the process taught in U.S. Pat. No. 4,002,562 to Amsu, the preferred amine, triethylamine, is removed from the oil-amine mixture by low temperature distillation, leaving behind a fixed oil. Triethylamine has a normal boiling point of 89.8℃ (vapor pressure = 760
mmHg). On the other hand, oils with molecular weights around 1000 have high boiling points, with initial distillation typically starting above 300°C and a smoke point of 200°C.
That's all.

When this oil-amine mixture is gently heated, for example by drying overnight at 105°C, about 20-30% by weight of triethylamine remains in the oil. This result is accurately predicted by Raoult's law. However, if the oil-amine mixture is heated to a temperature above which it begins to smoke, e.g. 200 DEG C., the triethylamine is not completely removed as expected. According to Raoult's law, heating the oil-amine mixture under these conditions will leave only about 0.8% by weight of the amine in the oil. However, in practice, about 8-15% by weight remains. When heated further, no amine remains, but on the contrary, the amine is decomposed.

Thus, known methods of removing amines from oil-amine mixtures are unsatisfactory. I mean,
These methods lead to loss of amine and contamination of the oil. Accordingly, there is a need for a process for removing amines from oil-amine mixtures without loss of amines and in which the resulting oil is substantially amine-free.

SUMMARY OF THE INVENTION It is therefore an object of the present invention to provide a method for removing amines from oil-amine mixtures that minimizes amine losses and reduces the concentration of residual amines in the oil. Our goal is to provide the following.

Furthermore, it is an object of the present invention to describe a unique arrangement of devices designed to facilitate the use and control of the methods described herein.

It is also an object of the present invention to provide a unique method for monitoring the steps necessary to perform the separation.

Yet another object of the present invention is to provide a method for removing amines from oil-amine mixtures using water and a method for controlling the amount of water required to perform such separation.

(Means for Solving the Problems) The present invention relates to a method of removing amines from oil-amine components produced by known methods using water, and in particular, the method of the present invention includes It is useful in conjunction with known methods of breaking emulsions and breaking up sludges containing oil, water and solid materials. The known method uses amines or mixtures thereof with inverted critical solution temperatures with water to carry out the separation. A method of breaking an emulsion comprising oil and water includes mixing the emulsion with an amine having an inverse critical solution temperature with water to form a single phase mixture, wherein the mixture has a temperature below the inversion critical solution temperature. After this step, increasing the temperature of the single phase mixture to a temperature above the inversion critical temperature of the amine to form a water component containing a small amount of amine and an oil-amine component containing a small amount of water. is included. The water component is then separated from the oil-amine component.

Known methods for destroying sludge containing oil, water and solid materials include mixing the sludge with an amine having an inverse critical solution temperature to that of water to form a mixture, wherein the mixture is It has a temperature below the inversion critical solution temperature of the amine. Below the inversion critical solution temperature of the amine, the solid material is separated from the mixture, leaving only a single phase mixture. Following this, the temperature of the single phase mixture is raised above the inverted critical solution temperature of the amine to obtain a water component containing a small amount of amine and an oil-amine component containing a small amount of water. The water component is then separated from the oil-amine component.

The amine used in the known method has an inverse critical solution temperature with water and has the following formula: (Here, R ₁ is hydrogen or an alkyl group,
R ₂ and R ₃ represent an alkyl group having 1 to 6 carbon atoms or an alkenyl group having 2 to 6 carbon atoms, and the preceding number of carbon atoms is 3 to 7.

One such amine is triethylamine.

The present invention relates to a process for removing amines from oil-amine components, such as those made by known methods such as those described above, using water. The present invention also discloses a method of controlling the amount of water required to perform such separation. In addition, the present invention also provides an apparatus for removing amines or mixtures thereof from oil-amine components using water to perform such separations and for controlling the amount of water required to perform this separation. An apparatus is also disclosed. The method of the present invention includes the step of adding water to the oil-amine component to form a water-oil-amine mixture, where the amount of water added covers substantially all of the amine in the oil-amine component. and water
in an amount sufficient to form an amine azeotrope),
and heating this water-oil-amine mixture to
including the step of removing the amine azeotrope. This step of adding water can be a step of adding liquid water or steam. The heating step can be carried out in a device that allows simultaneous heating and mass transfer. At least one of the mass transfer devices may be an evaporator, examples of which are rising film evaporators and falling film evaporators. Also, optionally in combination with an evaporator, the at least one mass transfer device can be a distillation column, such as a reboiled multi-stage distillation column. This heating step may include adding steam to the distillation column. Such water vapor addition provides not only heat but also water to the system. A variant of the process of the invention includes the step of heating the oil-amine component before adding water, the step of heating the oil-amine component being performed in a rising film evaporator or a falling film evaporator. An evaporator such as an evaporator can be used. The method of the present invention can be used to remove amines from oil-amine components even when the amount of amine in the oil-amine component is less than 10% by weight.

The method of the invention includes the step of determining whether the amount of water added is sufficient to form a water-amine azeotrope with substantially all of the amine in the oil-amine component. I can do it. Determining whether the amount of water added is sufficient may include measuring the amount of amine present in the oil-amine component, e.g. by gas chromatography and using e.g. a flow meter. measuring the amount of water added to the oil-amine. The step of determining whether the amount of water added is sufficient may also include the step of measuring the specific gravity of the water-oil-amine mixture before the heating step. The specific gravity of this water-oil-amine mixture will of course depend on the specific gravity of the oil. If the specific gravity of this oil is about 0.9,
and the amine is triethylamine, and a sufficient amount of water is added to the oil-amine component to form a water-amine azeotrope with substantially all of the amine in the oil-amine component; This water-oil-
The specific gravity of the amine mixture is about 0.73 at 135〓
It is 0.78.

The present invention also provides an alternative method for determining whether the amount of water added is sufficient. For example, if the heating step uses an evaporator, steam will flow out of the evaporator during the heating step. The temperature of the vapor leaving this evaporator gives an indication of the content of the vapor. When the temperature of the vapor is approximately equal to the boiling point of the water-amine azeotrope, the vapor exiting the evaporator consists essentially of the azeotrope. For example, if the amine is triethylamine, the temperature of the steam from the steamer is approximately
169-171〓 (about 76.1-about 77.2℃).

A similar method can be used when using a distillation column in the heating step. Steam is released from the distillation column during the heating process, and temperature measurements of the steam provide an indication of the steam composition. When the temperature of this vapor is approximately equal to the boiling point of the water-amine azeotrope, the vapor exiting the column consists essentially of the azeotrope. For example, if the amine is triethylamine, the temperature of the vapor from the distillation column is between about 175
185〓 (approximately 78.9~85℃). As explained in more detail below, the system is preferably operated by adding a slight excess of water to substantially completely remove the amine from the oil-amine component. The use of this slight excess of water is because the steam leaving the evaporator has a slightly higher temperature than the steam from the distillation column. Due to the use of excess water, the temperature of the steam coming out of the distillation column is 212
(100°C); such high temperatures indicate that the tower is uneconomical to operate.

Another method of determining whether the amount of water added is sufficient involves measuring the temperature of the oil left after the heating step to remove substantially all the water-amine azeotrope. . If the amount of water added is not sufficient, the temperature of the oil will rise significantly.

As noted above, the present invention can be used to remove amines from any oil-amine mixture, such as those produced by the known methods of breaking emulsions and sludges described above.

The present invention also includes an apparatus for removing amines from an oil-amine mixture, including a means for adding water to the oil-amine mixture to form a water-oil-amine mixture, an amount of water added, and an apparatus for removing amines from an oil-amine mixture. means for controlling the amount of water added to be sufficient to form a water-amine azeotrope with substantially all of the amine in the oil-amine mixture and the water-oil-amine mixture; and means for heating the mixture to form a water-amine azeotrope. The heating means may be one or more devices that allow mass transfer and heating at the same time. One such mass transfer device is an evaporator, such as a rising film evaporator or a falling film evaporator. Another such device is a distillation column, such as a reboiling multi-stage distillation column. For example, the heating means can include an evaporator and a multi-stage distillation column.

Means for controlling the amount of water added include means for measuring the amount of amine in the oil-amine mixture, such as a gas chromatograph, and means for measuring the amount of water added to the oil-amine component, such as a flow meter. be able to. The means to control the amount of water added is water-
A means for measuring the specific gravity of the oil-amine mixture may also be included. Furthermore, the means for controlling the amount of added water may also include means for simultaneously achieving heating and mass transfer, for example means for measuring the temperature of the vapor from the evaporator or distillation column.

The present invention uses water to remove amines from oil-amine components obtained by known methods of breaking emulsions and sludges using amines or mixtures thereof that have inverted critical solution temperatures with water. Regarding the method. The water in the sludge may be bound or unbound water. The term emulsion as used herein refers to water and animal,
Includes emulsions containing oils, greases, fats, fats, etc. of vegetable or petroleum origin. oil-
Includes emulsions of the water-in-water and oil-in-water types. The term sludge as used in the present invention encompasses emulsions as described above which contain solid substances, particularly in finely divided form. Some typical sludges include sewage sludge, petroleum sludge, and industrial sludge, including sludges that contain harmful compounds such as PCBs and
The Resource Conservation and Recovery Act (Resource Protection Agency)
Conservation and Recovery Act) KO01,
Includes sludge listed as hazardous wastewater in KO48, KO49, KO50, KO51 and KO52.

A known method for breaking emulsions containing oil and water involves warming the emulsion with an amine or a mixture thereof having an inverted critical solution temperature with water, and adjusting the temperature of the resulting mixture to the inverted critical solution temperature of the amine. Keep the temperature below the solution temperature. This mixture is more or less single phase. The temperature of this single phase mixture is then raised above the inverted critical solution temperature of the amine to form two components: a water component containing a small amount of amine and an oil-amine component containing a small amount of water. The water component is separated from the oil-amine component and optionally further processed or discarded.
The oil-amine component can be used in other known ways,
It may also be further processed as in the present invention.

Known methods for breaking sludge are very similar to those described above for emulsions, except for the following additional steps. After the amine is added to the sludge to form a mixture below the inversion critical solution temperature of the amine, the solid material is separated from the remainder of the mixture by known methods such as centrifugation or filtration. The remainder of this mixture is more or less single phase and contains water, oil, and amine. This water-oil-amine is typically treated as described above.

Preferred amines for the known process have an inverted critical solution temperature relative to water as described above. The most preferred conventional amines are those that exhibit an inverted critical solution temperature at about atmospheric pressure at ambient temperatures. Below this inversion critical solution temperature, water and amine are completely miscible in all proportions. Below this inversion critical solution temperature, the amine and water separate into two distinct phases, one composed primarily of the amine with a small amount of water, and the other phase containing a small amount of the amine. A phase consisting primarily of dissolved water.

More particularly, preferred amines of the known process include amines selected from the group of amines of the following formula or mixtures thereof: where R ₁ is hydrogen or an alkyl group, and R ₂
and R ₃ are each independently an alkyl group having 1 to 6 carbon atoms or an alkenyl group having 2 to 6 carbon atoms, and the total number of carbon atoms in the amine molecule is 3 to 7. Representative examples of these amines are triethylamine and diisopropylamine, with triethylamine being most preferred. The two-phase system of triethylamine and water is 760 mm
It is characterized by an inverted critical solution temperature of about 18.7°C (about 66〓) under the pressure of Hg.

The present invention uses water to separate the amine from the oil-amine component or mixture. A surprising feature of the present invention is that the present invention involves the addition of water at some point in the known method, whereas the end point of the prior art is separation of water. In the known method, most of the water has already been removed at that point. In the present invention, water is used to form an azeotrope with substantially all of the amines in the oil-amine mixture, and the azeotrope is separated from the oil by heating.

Although the objectives of the present invention can be achieved by simply adding water and heating to remove the water-amine azeotrope, the amount of water added can be controlled to maximize removal of the amine and at the same time remove the oil. It is desirable to minimize the amount of water left after separating the amine from the amine. A preferred embodiment of the invention achieves adequate control and is described below in accordance with FIG.

FIG. 1 schematically shows a preferred embodiment of the present invention. This oil-amine component stream enters at position 1. Liquid water 2 is added to this oil-amine component to form a water-oil-amine mixture that is transferred to analyzer 3. Using this analyzer is one way to determine whether enough water has been added. In a preferred embodiment of the invention, the analyzer measures the specific gravity of the water-oil-amine mixture. This measurement gives an indication of the amount of water in the water-oil-amine mixture. The specific gravity of the oil is about 0.9,
and the amine is triethylamine, and the amount of water added to the oil-amine component is sufficient to form an azeotrope with substantially all of the amine; The specific gravity of the components is preferably between 0.73 and 0.78 at 135°C (approximately 68.3°C). Other methods of determining the amount of water in the water-oil-amine mixture are also available, such as automated Karl Fischer titration to determine the water content of stream 4 or the water versus oil-amine component. flow 2 proportional to flow 1 to obtain a specific ratio of
Examples include, but are not limited to, actual measurement of the flow rate of stream 1 while controlling the flow of water within the stream. The water content of the water-oil-amine mixture in stream 4 is approximately 10% by weight of the amine content. This makes it possible to consider that all the amine is released from the heating system as an azeotrope.

The first means for heating this water-oil-amine mixture is a riser thin film evaporator 5 from which steam is released at point 7 during heating. other evaporators,
For example, falling film evaporators as well as other known evaporators can be used. Sufficient water is provided in stream 2 such that substantially all of the vapor released from the riser film evaporator at point 7 is a water-amine azeotrope and the temperature of this vapor is such that the temperature of the vapor is such that the water-amine azeotrope Approximately equal to the boiling point of the amine azeotrope. In the most preferred embodiment of the invention, the amine is triethylamine and the temperature of the vapor exiting at the seven positions is about 169-171° (76.1-77.2°C) at atmospheric pressure.

The water-oil-amine mixture rises at position 6 and is discharged from the thin film evaporator, and is discharged from the reboiling multi-stage distillation column 8.
Steam is released from there during heating at position 9. If enough water is added to stream 2 to form a water-oil-amine azeotrope, the temperature of the steam at position 9 will be approximately equal to or below the boiling point of the water-amine azeotrope. is also slightly higher. In the most preferred embodiment of the invention, the amine is triethylamine and the temperature at the top of tower 9 is about 175-185
〓 (approximately 78.9-85℃). In the most preferred embodiment, the vapor exiting the distillation column at position 9 contains an excess of water than required for the water-amine azeotrope. This is also a control measure used to ensure that substantially all amines are removed from the oil. Therefore, the temperature of the vapor from the distillation column is slightly higher than the temperature of the vapor from the evaporator in the most preferred embodiment.

Another means of ensuring nearly safe removal of amines from oil-amine mixtures is to add water vapor 11 to the still.
is to add. The addition of steam not only provides a heat source, but also helps ensure sufficient water addition. By monitoring the temperature of the steam released at position 9 and adjusting the distillation column by adding steam, an outlet temperature of 175-185〓 is guaranteed.
The system will operate to remove substantially all of the amine from the oil-amine mixture.

Heating of the reboiling column 8 is achieved indirectly by the reboiler 12. The oil is discharged from the tower at position 10, recycled through reboiler 12, heated indirectly in the reboiler, and then re-entered the tower to form the amine by azeotrope with water. further remove. When substantially all of the amines are removed, the oil is 14
, where the oil is recycled and used for any desired purpose. The oil at position 14 contains a small amount of water, but it is appropriately monitored with analyzer 3.
Moreover, by properly scanning the riser film evaporator and distillation column, including maintaining the outlet temperature appropriately and adding water vapor as necessary,
The oil from the position will contain only traces of water.

Stream 4, carefully monitored by analyzer 3, is maintained such that the water content is greater than 10% by weight of the amine content, so that substantially all of the amine is removed from the riser and thin film evaporator 5. It will be separated from the oil-amine component. Proper addition of water at position 2 and proper monitoring of water addition at position 3 also ensures that sufficient water is present in tower 8 without the need for addition of steam at position 11. , also guarantees complete removal of the amine as an azeotrope. However, preferred embodiments include the possibility of adding steam to ensure proper operation of the column and to almost completely remove the amine.

In addition to the addition of water at positions 2 and 11 previously mentioned, water can be injected at various other positions between 1 and 14 to effect amine removal and thereby practice the invention. Injection at position 15 is appropriate if energy conservation is a top priority. The amine will be removed in the evaporator as a nearly pure component by simply heating rather than being removed as an azeotrope. Overall, very little water will be introduced into this process. Therefore, a small amount of water must be evaporated. This can be an important energy consideration when comparing the relative energies required to evaporate amines and water.

Amine - ~130 BTU/lb; Water - ~950 BTU/lb.

Appropriate monitoring of the temperature at positions 9 and 10 is required to regulate the amount of water in the oil-amine component introduced into distillation column 8. As mentioned above, if the amount of water in this column is sufficient to almost completely form the azeotrope, the temperature at the top of column 9 will be approximately equal to the boiling point of the azeotrope. The temperature of the oil at position 10 is also an indicator of proper operation of the tower. When a sufficient amount of water is present in the oil, the temperature of the oil is kept lower than it would be if the oil did not contain water. By practicing the present invention, the amount of amine left in the oil is significantly less than the amount of amine left after practicing the known method.
Also, by practicing the present invention, the amount of water left in the oil is minimal and can be removed by known methods including polishing.

Liquid water can also be injected at various locations on the tower (including location 16). The heat input to the reboiler keeps the amount of water in the oil at a trace level. The amount of water injected at position 16 is measured with a flow meter, which makes it possible to ensure a proper balance of water to amine content.

Examples 1 Sludge from an operating oil refinery was treated with the above known method using triethylamine as the amine to obtain an oil-triethylamine mixture.
The oil-triethylamine mixture was heated to 100°C to remove triethylamine. The oil product was obtained after the removal of triethylamine was apparently complete. This oil was analyzed for residual triethylamine and was found to contain approximately 250,000 ppm or 25% by weight triethylamine. In an attempt to remove residual triethylamine,
The oil was ignited to the smoking point (above 200°C) and maintained at this temperature for approximately 30 minutes. According to the analysis,
It was found that 80,000 ppm or 8% by weight of triethylamine remained.

2 Sludge from an operating oil refinery was treated with the above known method using triethylamine as the amine to produce an oil-triethylamine mixture. In the laboratory, liquid water was added to the oil-triethylamine mixture. The amount has a specific gravity of approximately 0.73
The amount was such that it was ~0.78. The water-oil-triethylamine mixture was then heated to remove triethylamine as an azeotrope with water. After distillation, residual triethylamine in the oil is
It was less than 400 ppm, or 0.04% by weight.

From the foregoing description, aspects of the invention have been described for purposes of disclosure; however, various changes can be made without departing from the spirit and scope of the invention.
Accordingly, the invention is not limited except as by the scope of the claims appended hereto.

[Brief explanation of the drawing]

Attached FIG. 1 is a diagram schematically showing the apparatus of the present invention, which includes a step of adding water, a heating step, and a step of measuring whether the amount of added water is sufficient. The steps of the inventive method are shown. (Main reference numbers), 2...Liquid water, 3...Analyzer, 5...Rising thin film evaporator, 8...Reboiling multi-stage distillation column, 9...Distillation column top, 12...Refill Boiler.

Claims (1)

[Claims] 1. A method for breaking an emulsion containing oil and water, comprising the following steps: An amine having an inverse critical solution temperature with water is mixed with the emulsion to form a single-phase mixture (the mixture has a temperature below the inverted critical solution temperature of said amine), and raising the temperature of said mixture above the inverted critical solution temperature of said amine to form an aqueous component containing a small amount of amine and a small amount of water. and separating the water component from the oil-amine component, the method comprising: adding water to the oil-amine component to form a water-oil-amine mixture. forming a water-amine azeotrope with substantially all of the amine in the oil-amine component; and -Heating the amine mixture to produce the water-
removing an amine azeotrope. A method for removing the amine from the oil-amine component. 2. The method of claim 1, wherein the heating step uses at least one device for simultaneous heating and mass transfer, the device being an evaporator or a distillation column. 3 further comprising the step of determining whether the amount of water added is sufficient to form a water-amine azeotrope with substantially all of the amine in the oil-amine component. The method described in Section 1. 4. The step of determining whether the amount of water added is sufficient comprises measuring the amount of amine present in the oil-amine component and measuring the amount of water added. Method described. 5. The method of claim 3, wherein the step of determining whether the amount of water added is sufficient includes the step of measuring the specific gravity of the water-oil-amine mixture before the heating step. 6. The heating step uses an evaporator that produces steam,
4. The method of claim 3, wherein the step of adding water includes adding enough water such that the temperature of the vapor exiting the evaporator is approximately equal to the boiling point of the water-amine azeotrope. 7. The heating step uses a multi-stage distillation column from which steam is produced, and the water addition step uses a temperature sufficient to make the temperature of the steam coming out of the multi-stage distillation column substantially equal to the boiling point of the water-amine azeotrope. 4. The method of claim 3, including the step of adding water. 8. A method for destroying a sludge containing oil, water, and a solid substance, comprising the following steps: Mixing the sludge with an amine having an inverted critical solution temperature relative to water (the mixture is a mixture of the amine and the amine). (having a temperature below the inversion critical solution temperature)
separating the solid material from the mixture to leave a single phase mixture at a temperature below the inverted critical solution temperature of the amine; and bringing the temperature of the single mixture above the inverted critical solution temperature of the amine. a water component containing a small amount of amine and an oil-amine component containing a small amount of water; and a step of separating the water component and the oil-amine component. Step: Adding water to the oil-amine component to form a water-oil-amine mixture (however, the amount of water added is such that a water-amine azeotrope is formed with substantially all of the amine in the oil-amine component). and heating the water-oil-amine mixture to remove the water-amine azeotrope. A method of using water to 9. A method according to claim 8, wherein the heating step uses at least one device allowing simultaneous heating and mass transfer, the device being an evaporator or a distillation column. 10. Claim further comprising the step of determining whether the amount of water added is sufficient to form a water-amine azeotrope with substantially all of the amine in the oil-amine component. 8. The method described in 8. 11. Said step of determining whether the amount of water added is sufficient comprises the steps of measuring the amount of amine present in said oil-amine component and measuring the amount of water added. The method according to item 10. 12. Claim 1, wherein the step of determining whether the amount of water added is sufficient includes the step of measuring the specific gravity of the water-oil-amine mixture before the heating step.
The method described in 0. 13. The heating step uses a steam-producing evaporator, and the water addition step adds enough water such that the temperature of the steam exiting the evaporator is approximately equal to the boiling point of the water-amine azeotrope. Claim 10 comprising the step
Method described. 14. The heating step uses a steam-producing distillation column, and the water addition step adds enough water such that the temperature of the steam exiting the distillation column is approximately equal to the boiling point of the water-amine azeotrope. Claim 1 including the step
The method described in 0. 15 An apparatus for removing an amine from an oil-amine mixture, the apparatus comprising: adding water to the oil-amine mixture to form a water-oil-
means for forming an amine mixture; and adding water such that the amount of water added is sufficient to purify the water-amine azeotrope with substantially all of the amine in the oil-amine mixture. An apparatus comprising: means for controlling the amount of water; and means for heating the water-oil-amine mixture to purify a water-amine azeotrope. 16. Apparatus according to claim 15, wherein the heating means comprises one or more devices allowing simultaneous heating and mass transfer, at least one of which is an evaporator or a distillation column. 17. The apparatus of claim 15, wherein said means for controlling the amount of water added includes means for measuring the amount of amine present in said oil-amine mixture and means for measuring the amount of water added. 18. The apparatus of claim 15, wherein said means for controlling the amount of water added includes means for measuring the specific gravity of said water-oil-amine mixture. 19. The apparatus of claim 16, wherein said means for controlling the amount of water added includes means for measuring the temperature of steam discharged from said evaporator. 20. The apparatus of claim 16, wherein said means for controlling the amount of water added includes means for measuring the temperature of the steam exiting said distillation column.