CA2074031A1 - Method and device for recovering glycol(s) from a mixture of glycol(s) and water - Google Patents

Method and device for recovering glycol(s) from a mixture of glycol(s) and water

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Publication number
CA2074031A1
CA2074031A1 CA002074031A CA2074031A CA2074031A1 CA 2074031 A1 CA2074031 A1 CA 2074031A1 CA 002074031 A CA002074031 A CA 002074031A CA 2074031 A CA2074031 A CA 2074031A CA 2074031 A1 CA2074031 A1 CA 2074031A1
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Canada
Prior art keywords
reservoir
piping
water
ethylene glycol
mixture
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Abandoned
Application number
CA002074031A
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French (fr)
Inventor
Benny Dobrofsky
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Individual
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Individual
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Priority to CA002074031A priority Critical patent/CA2074031A1/en
Publication of CA2074031A1 publication Critical patent/CA2074031A1/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/88Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/26Treatment of water, waste water, or sewage by extraction
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/94Use of additives, e.g. for stabilisation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

ABSTRACT OF THE DISCLOSURE:

The present invention relates to a method for recovering glycol(s), especially ethylene glycol, from a mixture of glycol(s) and water. This method comprises the following steps: admixing in a first reservoir a mixture of glycol(s) and water with a sufficient amount of a compound reacting with water to give a product insoluble inwater and form a slurry which is defined as a suspension of at least said insoluble product in water and in which glycol(s) are insoluble; allowing the mixture obtained from the preceding step to separate into two distinct phases, that is an upper phase essentially consisting of glycol(s) and a lower phase essentially consisting of the above mentioned slurry, said phases being separated by an interface glycol(s) - slurry;
collecting the lower phase contained in the first reservoir and carrying it into a second reservoir; and collecting the upper phase of the first reservoir and carrying it into a third reservoir; glycol(s) of the third reservoir being ready to be used, while the slurry of the second reservoir is ready to define a valuable by-product. The invention also relates to a device usable to carry out this method.

Description

- 2n7~03l ~ETHOD I~ND DEYICE FOEI RECOVERIN(: GLYCOL ( S ) FROM A MIXTURE OF GLYCOL ( S ) WITH WATER

BACRGROUND OF THE INVENTION

a ! Field of the invention The present invention relates to a method and a device for recover~ng glycol(s) from a mixture of glycol(s) and water, especially ethylene glycol from a mixture of ethylene glycol and water obtained after having used ethylene glycol for de-icing aircrafts at an airport.

b) Brief description of the prior art Glycols are compounds that are frequently mixed with water (e.g. cooling mixtures). Also, after having de-iced an aircraft with ethylene glycol, a mixture of water and ethylene glycol (especially a mixture of about 10 to 20% of ethylene glycol and of 90 to 80% of water) is obtained.
This mixture is then either allowed to drain into sewer systems of the airport and discharge in rivers, or to penetrate in the soil. However, ethylene glycol is well known to be poisonous and therefore when discharged in rivers or allowed to penetrate in the soil, it contaminates water and/or the water table to thus endanger the health of citizens.
Methods actually known for recovering glycols, especially ethylene glycol, are generally carried out with chemical processes where there is an economical interest to recycle ethylene glycol to previous steps of said processes or to remove ethylene glycol from a final product in order to embody a product having determined characteristics.
To the applicant's knowledge, there was never 2074~3~

taught to separate ethylene glycol from an a~ueous mixture thereof according to a method that is simple and unexpensive, especially in order to re-use ethylene glycol for de-icing aircrafts at an airport. ( For example, an airport such as Dorval airport near Montréal (Canada) spent each year more than $100 000 of ethylene glycol.) Therefore, there is a strong need for a simple and unexpensive method and a device allowing to recover glycol(s), especially ethylene glycol, from a mixture of glycol(s) and water.

STJMMARY OF TEIE INVENTION

The present invention relates to a method for recovering glycols from a mixture of glycol(s) and water, and especially ethylene glycol from a mixture of ethylene glycol and water obtained after having used ethylene glycol for de-icing aircrafts. This process comprises the following steps:
- Admixing in a first reservoir a mixture of glycol(s) and water with a sufficient amount of a compound reacting with water to give a product insoluble in water and forming a slurry in which at least said insoluble product is suspended and in which glycol(s) are insoluble.
- Allowing the mixture obtained from the preceding step to separate into two distinct phases, that is an upper phase essentially consisting of glycol(s) and a lower phase essentially consisting of the above mentioned slurry, said phases being separated by an interface glycol(s) - slurry.
- Collecting at least a part of the lower phase contained in the first reservoir and carrying it into a second reservoir.
- Collecting at least a part of the upper phase of the first reservoir and carrying it into a third 2~7~031 reservoir~
Glycol(s) of the third reservoir are ready to be used, while the slurry of the second reservoir is ready to define a valuable by-product ( e.g. a by-product suitable to be delivered to industries as a base for neutralizing acids, in cement mixtures, ect.).
Advantageously, glycol(s) may consist of ethylene glycol.
More particularly, the present invention relates lo preferably to a method for recovering ethylene glycol from a mixture of ethylene glycol and water obtained after having used ethylene glycol for de-icing an aircraft. This method comprises the following steps:
- Collecting a mixture of ethylene glycol and water running off from an aircraft when ethylene glycol is applied against it to melt ice formed thereon.
- Carrying said mixture of ethylene glycol and water into a first reservoir.
- Admixing the mixture of ethylene glycol and water contained in the first reservoir with a sufficient amount of a compound reacting with water to give a product insoluble in water and forming a slurry in which at least said insoluble product is suspended and in which ethylene glycol i8 insoluble.
- Allowing the mixture obtained from the preceding step to separate into two distinct phases, that is an upper phase essentially consisting of ethylene glycol, and a lower phase essentially consisting of the above mentioned a slurry, said phases being separated by an interface ethylene glycol - slurry.
- Collecting at least a part of the lower phase contained in the first reservoir and carrying it into a second reservoir.
- Collecting at least a part of the upper phase of the first reservoir and carrying it into a third 2~7~031 reservoir.
The ethylene glycol of the second reservoir is ready to be used for de-icing another aircraft, while the slurry of the third reservoir is ready to define a valuable by-product ( e.g. a by-product suitable to be delivered to industries aæ a base for neutralizing acids, in cement mixtures, ect.).
Advantageously, the compound intended to react with the water of the mixture of glycol(s) and water, especially of the mixture of ethylene glycol and water, is selected from the group consisting of alkali oxides and alkali earth oxides, preferably a calcium oxide such as lime. According to a particularly preferred embodiment of the invention, the compound is a powdered lime ( CaO ).
This compound reacts with water according to the following equation:
CaO + H2O -~ Ca(OH)2 The original mixture of glycol(s), especially ethylene glycol, and water will separate because glycol(s), especially ethylene glycol, are insoluble in a slurry containing an alkali or alkali-earth hydroxide, especially a slurry containing lime water (i.e. Ca(OH)2).
The invention also relates to a device ~or recovering glycol(s) from a mixture of glycol(s) and water wherein it comprises:
- a first, a second and a third reservoirs;
- means for filling the first reservoir with a mixture of glycol(s) and water;
- means for introducing and admixing with the mixture of glycol(s) and water contained in the first reservoir, a sufficient amount of a compound ~advantageously lime and preferably lime in excess) intended to react with water of said mixture, give a 207~a3l product insoluble in water and form a slurry in which at least said insoluble product is suspended and in which glycol(s) are insoluble (advantageously a slurry comprising lime water and preferably a slurry comprising lime and lime water);
- means allowing the mixture of glycol(s~ and slurry to separate into two distinct phases, that is an upper phase essentially consisting of glycol(s) and a lower phase essentially consisting of the above mentioned slurry;
lo - means for collecting and carrying the lower phase into the second reservoir, said means being located below the interface glycol(s) - slurry;
- means for collecting and carrying the upper phase into the third reservoir,.said means being located above the interface glycol(s) - slurry.
More particularly, the present invention relates to a device for recovering ethylene glycol from a mixture of ethylene glycol obtained after having used ethylene glycol for de-icing an aircraft. This device comprises:
- a first, a second and a third reservoirs;
- means for collecting a mixture of ethylene glycol and water running off the a~rcraft when ethylene glycol is applied to melt lce ~ormed thereon;
- means for carrying said collected mixture of ethylene glycol and water, into the first reservoir;
- means for introducing and admixing with the mixture of ethylene glycol and water contained in the first reservoir, a sufficient amount of a compound (advantageously lime and preferably lime in excess) intended to react with water of the mixture, give a product insoluble in water and form a slurry in which said insoluble product is suspended and in which ethylene glycol is insoluble (advantageously a slurry comprising lime water and preferably a slurry comprising lime and lime water ~;
- means allowing the mixture of ethylene glycol 207~31 and above mentioned slurry to separate into two distinct phases, that is an upper phase essentially consisting of ethylene glycol, and a lower phase essentially consisting of the above mentioned slurry (advantageously a slurry comprising lime water and preferably a slurry comprising lime and lime water);
~ means for collecting and carrying the lower phase into the second reservoir, (advantagsously a slurry comprising lime water and preferably a slurry comprising lime and lime water);
- means for collecting and carrying the upper phase into the third reservoir.

BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be better understood with reference to the following non-restrictive description of a preferred embodiment thereof, taken in connection with the following drawings:
Figure 1 represents a schematic view of a device for recovering a glycol(s) from a mixture of glycol(s) and water;
Figure 2 represents a schematic view of a device for recovering ethylene glycol from a mixture of ethylene glycol and water obtained after having used ethylene glycol ~or de-icing an aircraft.

DESCRIPTION OF PREFERRED EMBODIMENTS

Referring to Figure 1 there is represented a schematic view of a device for recovering glycol(s) from a mixture of glycol(s) and water.
This device "D" comprises:
- a first reservoir 1, a second reservoir 3 and a third reservoir 5;

2 1) 7 ~

- means 7 for filling the first reservoir 1 with a mixture of glycol(s) and water;
- means 9,10 for introducing and admixing with the mixture contained in the first reservoir 1, a sufficient amount of a compound (advantageously lime and preferably an excess of lime) intended to react with water of the mixture to give a product insoluble in water and form a slurry in which at least said insoluble product is suspended and in which glycol(s) are insoluble (advantageously a slurry comprising lime water and preferably a slurry in which lime and lime water are suspended) and means allowing the mixture obtained from the preceeding step to separate into two distinct phases, that is an upper phase 11 essentially consisting of glycol(s) and a lower phase 13 essentially consisting of the above mentioned slurry (advantageously a slurry comprising lime water and preferably a slurry comprising lime and lime water), said phases being separated by an interface 21 glycol(s) - slurry;
- means 17 for collecting and carrying the lower phase 13 into the second reservoir 3;
- means 19 for collecting and carrying the upper phase 11 into the third reservoir 5;
Advantageously, means 7 for filling the first reservoir 1 with a mixture of glycol(s) and water consist of a first piping 203 having opposite ends, one end of said piping being intended to be in contact with a mixture of glycol(s) and water while the opposite end thereof is connected to the first reservoir 1. This first piping 203 may further comprises a pump 205 and /or a valve 206.
Advantageously, means 9 for introducing a compound intended to react with water of the mixture to give a product insoluble in water, form a slurry in which the insoluble product is suspended and in which glycol(s) is insoluble, consist of a bin 211 located above and 2074~31 communicating with an interior 213 of the first reservoir 1 ~said bin may preferably contain powdered lime); means for admixing the compound with the mixture o~ glycol(s) and water consist of an air injector 207 having opposite ends, one end thereof being connected to the outlet of an air compressor 209 while the opposite end is positioned near the bottom of the first reservoir to thus bubble air in the first reservoir; and means for allowing the mixture of glycol(s) and the slurry to separate into two distinct phases consist of stopping the bubbling of air in the first reservoir. Of course, if desired, the air injector 207 may be replaced by a mechanical propeller dipped in the first reservoir 1 and driven by an electric motor.
Advantageously, means 17 for collecting and carrying the lower phase 13 in the second reservoir 3 consist of a second piping 221 having opposite ends, one and of said second piping 221 being connected to the bottom of the first reservoir 1 while the opposite end thereof is connected to the second reservoir 3. This second pipin~ 221 may further comprises a pump 223 and/or a valve 224.
Optionally, means for mixing the content of the second reservoir 3 may be provided. ~n example of such means may consist of an air injector 208 having opposite ends, one end thereof being connected to the outlet of an air compressor 210 while the opposite end is positioned near the bottom of the third reservoir 3 to thus allow bubbles of air to mix the content of said reservoir 3.
Advantageously, means 19 for collecting and carrying the upper phase 11 in the third reservoir 5 consist of a third piping 241 having opposite ends, one end of said third piping 241 being connected to a portion of the first reservoir 1 that is located above an interface 21 slurry - glycol(s), while the opposite end thereof is connected to the third reservoir 5. This third piping 241 may furthex comprises a pump 243 and/or a valve 244. Of 2Q7~03~

course, even though glycol(s) contained in the third reservoir may be re-used as such, it is possible to submit, if desired, said glycol(s) to one or several further purification steps well known to a skilled workman. For example only, glycol(s) may be subjected to a purge with carbon dioxide and then filtered.
Advantageously, the second reservoir 3 and third reservoir 5 are each further provided with means allowing to recover their content.
Preferably, the second reservoir 3 is further provided with a fourth piping 261 having opposite ends, one end of said fourth piping 261 being connected with the bottom of the second reservoir 3 while the opposite end thereof is connected to a valve 263. This fourth piping 261 15 may further comprises a pump 265.
Advantageously, the third reservoir 5 is further provided with a fifth piping 281 having opposite ends, one end of said fifth piping 281 being connected with the bottom of the third reservoir 5 while the opposite end 20 thereof is connected to a valve 283. This fifth piping 181 may further comprises a pump 285.
Referring to Figure 2 there is represented a schematic view o~ a device "DA" for recovering ethylene glycol from a mixture of ethylene glycol and water obtained 25 after having used ethylene glycol for de-icing an aircraft, said device comprising:
- a first reservoir 51, a second reservoir 53 and a third reservoir 55;
~ - means 57 for collecting a mixture of ethylene 30 glycol and water running off the aircraft when ethylene glycol is applied to melt ice formed thereon;
- means 59 for carrying said collected mixture of ethylene glycol and water, into the first reservoir 51;
- means 61,62 for introducing and admixing with 35 the mixture contained in the first reservoir 51, a compound 2074~31 intended to react with water of said mixture to give a product insoluble in water and form a slurry in which at least said insoluble product is suspended and in which ethylene glycol is insoluble, and means allowing the mixture obtained in the preceeding step to separate into two diætinct phases, that is an upper phase 63 essentially consisting of ethylene glycol, and a lower phase 65 essentially consisting of the above mentioned slurry;
- means 67 for collecting and carrying the lower phase 65 into the second reservoir 53.
- means 69 for collecting and carrying the upper phase 63 into the third reservoir 55.
Advantageously, means 57 for collecting the mixture of ethylene glycol and water running off from an airplane "A" consists of an existing sewage collector 101;
and means 59 for carrying said mixture in the first reservoir 51 consist of a first piping 103 (represented in part) having opposite ends, one end of said piping being connected to said sewage collector 101 while the opposite end thereof i8 connected to the first reservoir 51. This first piping 103 may furthe~ comprises a pump 105 and/or a valve 106.
Advantageously, means for introducing a compound intended to react with water of the mixture to give a product insoluble in water, form a slurry in which the insoluble product is suspended and in which glycol(s) is insoluble, consist of a bin 111 located above and communicating with an interior 113 of the first reservoir 1, said bin 111 may preferably contain powdered lime; means for admixing the compound with the mixture of glycol(s) and water consist of an air injector 107 having opposite ends, one end thereof being connected to the outlet of an air compressor 109 while the opposite end is positioned near the bottom of the first reservoir to thus bubble air in the first reservoir; and means for allowing the mixture of 207~3~

glycol(s) slurry to separate into two distinct phases consist of stopping the bubbling of air in the first reservoir. Of course, if desired, the air injector may be replaced by a mechanical propeller dipped in the first reservoir 1 and driven by an electric motor.
Advantageously, means 67 for collecting and carrying the lower phase 65 in the second reservoir 53 consist of a second piping 121 having opposite ends, one end of said second piping 121 being connected to the bottom of the first reservoir 51 while the opposite end thereof is connected to the second reservoir 53. This second piping 121 may further comprising a pump 123 and/or valve 124.
Optionally, means for mixing the content of the second reservoir 53 may be provided. An example of such means may consist of an air injector 108 having opposite ends, one end thereof being connected to the outlet of an air compressor 110 while the opposite end is positioned near the bottom of the third reservoir 53 to thus allow bubbles of air to mix the content of said reservoir 53.
Advantageously, means 69 for collecting and carrying the upper phase 63 in the third reservoir 55 consist of a third piping 141 having opposite ends, one end of said third piping 141 being connected to a portion of the first reservoir 51 that is located above an interface 71 slurry - ethylene glycol, while the opposite end thereof is connected to the third reservoir 55. This third piping 141 may further comprising a pump 143 and/or a valve 14~.
Of course, even though glycol(s) contained in the third reservoir may be re-used as such, it is possible to su~mit, if desired, said glycol(s) to one or several further purification steps well known to a skilled workman. For example only, glycol(s) may be subjected to a purge with carbon dioxide and then filtered.
Advantageously, the second reservoir 53 and third reservoir 55 are each further provided with means allowing 207~031 to recover their content.
Preferably, the second reservoir 53 is further provided with a fourth piping 161 having opposite ends, one end of said fourth piping 161 being connected with the bottom of the second reservoir 53 while the opposite end thereof is connected to a valve 163. This fourth piping 161 may further comprises a pump 165.
Advantageously, the third reservoir 55 is further provided with a fifth piping 181 having opposite ends, one end of said fifth piping 181 being connected with the bottom of the third reservoir 55 while the opposite end thereof is connected to a valve 183. This fifth piping 181 may further comprising a pump 185.
In order to use a device "D" as defined hereinbefore, the following steps are preferably carried out:
- Admixing in a first reservoir 1 a mixture of glycol(s), especially ethylene glycol, and water, with a compound (advantageously lime and preferably lime in excess~ intended to react with water to give a product insoluble in water and form a slurry (advantageously a slurry comprising lime water and preferably a slurry comprising lime and lime water) in which at least said insoluble product is suspended and glycol(s), especially ethylene glycol, is insoluble. The filling of the first reservoir 1 with a mixture of glycol(s), especially ethylene glycol, and water may be achieved when the piping 203 has one end thereof dipped or connected to a supply of a mixture of glycol(s), especially ethylene glycol, and water, the pump 205 is started and the valve 206 is opened.
To stop the filling, above steps just have to be reversed.
The introdu~tion of the compound in the mixture of glycol(s) and water may be achieved with a bin 211 usually provided with a trap 212 and containing said compound. To introduce said compound in the first reservoir it is just 2074~31 necessary to open said trap 212 and allow an amount of compound to drop by gravity in the first reservoir 1. To stop the introduction of compound, above steps just have to be reversed. Then, mixing of the mixture of glycol(s) and 5 water with the compound may be achieved when the air compressor 209 is started to allow bubbles of air to be injected in the first reservoir and create bubbles mixing the resulting mixture. To stop the mixing, above steps just have to be reversed.
- Allowing the mixture of glycol(s), preferably ethylene glycol, and water to separate into two distinct phases, that is an upper phase 11 essentially consisting of glycol(s), especially ethylene glycol, and a lower phase 13 essentially consisting of a slurry (advantageously a slurry comprising lime water and preferably a slurry comprising lime and lime water), said phases being thus separated by an interface 21 glycol(s) - slurry, especially ethylene glycol - slurry (advantageously a slurry comprising lime water and preferably a slurry comprising lime and lime water). This may be preferably achieved when the mixing with air bubbles is stopped.
- Collecting the lower phase 13 contained in the first reservoir 1 and carrying it into a second reservoir 3. This may be preferably achieved with piping 221 when the pump 223 is started and the valve 224 is opened. To stop this collection, above steps just have to be reversed.
- Collecting the upper phase 11 of the first reservoir 1 and carrying it into a third reservoir 5;
glycol(s), especially the ethylene glycol, of the third reservoir 3 being ready to be used, while the slurry (advantageously a slurry comprising lime water and preferably a slurry comprising lime and lime water) of the second reservoir 3 is ready to define a valuable by-product. This may be preferably achieved with piping 241 when the pump 243 is started and the valve 244 is opened.

207~031 To stop this collection, above steps just have to be reversed.
In order to use a device "DA" for recovering ethylene glycol from a mixture of ethylene glycol and water obtained after having used ethylene glycol for de-icing an aircraft, a method comprising the following steps may be carried out:
- Collecting a mixture of ethylene glycol and water running off the aircraft "A" when ethylene glycol is lo applied to melt ice formed thereon.
- Carrying said mixture of ethylene glycol and water, into a first reservoir 51. This may be acheived with piping 103, when the pump 105 is started and the valve 106 is opened. To stop this operation, above steps just have to be reversed.
- Admixing a suff~c~ent amount of a compound intended to react with water to give a product insoluble in water and form a slurry in which at least said insoluble product is suspended and ethylene glycol is insoluble. The introduction of the compound in the mixture of ethylene glycol and water may be achieved with a bin 111 usually provided with a trap 112 and containing said compound. To introduce said compound in the first reservoir it is just necessary to open said trap 112 and allow an amount of compound to drop by gravity in the first reservoir 51. To stop the introduction of compound, above steps just have to be reversed. Then, mixing of the mixture of glycol(s) and water with the compound may be achieved when the air compressor 109 is started to allow bubbles of air to be injected in the first reservoir and create bubbles mixing the resulting mixture. To stop the mixing, above steps just have to be reversed.
- Allowing the mixture obtained from the preceeding step to separate into two distinct phases, that is an upper phase 63 essentially consisting ethylene 2~7~31 glycol, and a lower phase 65 essentially consisting of the above mentioned slurry, said phases being thus separated by an interface 71 ethylene glycol - slurry ( this step is preferably achieved by mere stopping of the mixing step );
- Collecting the lower phase 65 contained in the first reservoir 51 and carrying it into a second reservoir 53. This may be preferably achieved with piping 121 when the pump 123 is started and the valve 124 is opened. To stop this collection, above steps just have to be reversed.
Preferably, air may be bubbled in the second reservoir 53 to avoid settling of their content, with an air injector 208 connected to an air compressor 210.
- Collecting the upper phase 63 of the first reservoir 51 and carrying it into a third reservoir 55;
15 the ethylene glycol of the third reservoir 55 being ready to be used, especially for de-icing another aircraft, while the slurry of the second reservoir 53 is ready to define a valuable by-product. This may be preferably achieved with piping 141 when the pump 143 is started and the valve 144 20 is opened. To stop this collection, above steps just have to be reversed.
Advantageously, the compound is lime (i.e.
calcium oxide), preferably powdered lime, and the valuable by-product is an aqueous slurry of calcium hydroxide and, 25 more preferably, of calcium hydroxide and lime.
Advankageously, lime is admixed with water in a ratio of at least 1:1 in the first reservoir 1 or 51.
Preferebly, an excess of lime ( for example in amount varying from 1~ to 2 times the weigh of water ) is admixed 30 with water in the first reservoir 1 or 51.
Advantageously, in the method using the device ''DA'I, the collection of the mixture of ethylene glycol and water running off from an airplane "A" is carried out with an existing sewage collector 101; and carrying of said 35 mixture in the first reservoir 51 is achieved with a first 207~

piping 103 having opposite ends, one end of said piping 103 being connected to said sewage collector 101 while the opposite end thereof is connected to the first reservoir 51, said first piping 103 further comprising a pump 105.
Advantageously, the admixing of lime with the mixture of glycol(s) and water or ethylene glycol and water is achieved with an air injector 207 or 107 dipped in the first reservoir 1 or 51 and connected to an air compressor 2~9 or 109.
Advantageously, the collection of the lower phase 13 or 65 of the first reservoir 1 or 51 is acheived with a second piping 221 or 121 having opposite ends, one end of said second piping 221 or 121 being connected to the bottom of the first reservoir 1 or 51 while the opposite end thereof is connected to the second reservoir 3 or 53, said second piping 221 or 121 further comprising a pump 223 or 123.
Advantageously, the collection of the upper phase 11 or 63 of the first reservoir 1 or 51 is acheived with a third piping 241 or 141 having opposite ends, one end of said third piping 241 or 141 being connected to a portion of the fir6t reservoir 1 or 51 that is located above an inter~ace 21 glycol(S) - slurry or 71 ethylene glycol -slurry, while the opposite end thereof is connected to the third reservoir 5 or 55, said third piping 241 or 141 further comprising a pump 243 or 143.

EXPERIMENTATION

A non limitative experimention has been carried out to illustrate the method making the object of the present invention. At this end, it was decided to separate ethylene glycol from a mixture of ethylene glycol and water.
apparatus:

207~031 2 x 10 ozs clear bottles with caps;
1 oz of ethylene glycol;
1 oz of H2O;
2 ozs of automobile radiator fluid (50% ethylene glycol, s 50% water);
2 x 2 ozs of powdered lime.
rocedure:
In one bottle, the dry powdered lime is measured by marking the top of the lime surface. Then, a mixture resulting from the admixion of 1 oz of ethylene glycol with 1 oz of H2O is added to the bottle containing the powdered lime. Then, the bottle is capped closed and shaked for about 2 minutes. Then, in about 15 minutes is settled into two phases, an upper phase that is clear and viscous, and a lower phase defining a slurry of lime water.
In the other bottle, the dry powdered lime is measured by marking the top of the lime surface. Then, a mixture resulting from the admixion of 2 ozs of an automobile radiator anti-freeze fluid containing 50%
ethylene glycol and 50% H2O, is added to the bottle containing the powdered lime. Then, the bottle is capped closed and shaked for about 2 minutes. Then, in about 15 minutes is settled into two phases, an upper phase that is clear and viscous, and a lower phase defining a slurry of lime water.
observations:
It took about 15 minutes for separation. The upper phase was clear and viscous, in volume equaling the amount of ethylene glycol used. The lower phase was a white slurry greater in volume than the amount of dry lime used.
With the automobile radiator anti-freeze fluid, the upper phase was yellow in color as the original mixture but only ~ the original volume of the 2 ozs used. This upper phase is viscous, the bottom slurry remains white.

2~7~031 conclusions:
Using powdered lime make possible to separate ethylene glycol from a mixture of ethylene glycol and water. The uppper phase is ethylene glycol. It is possible that some water remains in that phase but essentially almost all ethylene glycol of aforesaid mixtures have been recovered.
Of course, all aforesaid pumps, valves, pipings, reservoirs air injectors and air compressors used to embody the present invention are those well known individually to a skilled workman and do not mecessitate any detailled description. Furthermore, it should be noter that the invention also relates to all variations that may be obvious to a skilled workman.

Claims (27)

1. A method for recovering glycol(s) from a mixture of glycol(s) and water, wherein it comprises the following steps:
- admixing in a first reservoir a mixture of glycol(s) and water with a sufficient amount of a compound reacting with water to give a product insoluble in water and forming a slurry in which at least said insoluble product is suspended and in which glycol(s) are insoluble;
- allowing the mixture obtained from the preceding step to separate into two distinct phases, that is an upper phase essentially consisting of glycol(s) and a lower phase essentially consisting of the above mentioned slurry, said phases being separated by an interface glycol(s) - slurry;
- collecting at least a part of the lower phase contained in the first reservoir and carrying it into a second reservoir; and - collecting at least a part of the upper phase of the first reservoir and carrying it into a third reservoir;
glycol(s) of the third reservoir being ready to be used, while the slurry of the second reservoir is ready to define a valuable by-product.
2. A method for recovering ethylene glycol from a mixture obtained after having use ethylene glycol for de-icing aircrafts, wherein it comprises the following steps:
- collecting a mixture of ethylene glycol and water running off from an aircraft when ethylene glycol is applied against it to melt ice formed thereon;
- carrying said mixture of ethylene glycol and water into a first reservoir;
- admixing the mixture of ethylene glycol and water contained in the first reservoir with a sufficient amount of a compound reacting with water to give a product insoluble in water and forming a slurry in which at least said insoluble product is suspended and in which ethylene glycol is insoluble;
- allowing the mixture obtained from the preceding step to separate into two distinct phases, that is an upper phase essentially consisting of ethylene glycol, and a lower phase essentially consisting of the above mentioned a slurry, said phases being separated by an interface ethylene glycol - slurry;
- collecting at least a part of the lower phase contained in the first reservoir and carrying it into a second reservoir; and - collecting at least a part of the upper phase of the first reservoir and carrying it into a third reservoir;
the ethylene glycol of the second reservoir being ready to be used for de-icing another aircraft, while the slurry of the third reservoir is ready to define a valuable by-product.
3. A method according to claim 2, wherein the compound is selected from the group consisting of alkali oxides and alkali earth oxides.
4. A method according to claim 3, wherein the compound is a powdered lime ( i.e. calcium oxide ) and the valuable by-product is an aqueous slurry of calcium hydroxide.
5. A method according to claim 4, wherein lime is admixed with water of the mixture of ethylene glycol and water in a ratio of at least 1:1 in the first reservoir.
6. A method according to claim 5, wherein an excess of lime is admixed with water in the first reservoir, and wherein the unreacted portion of lime is suspended in the slurry.
7. A method according to claim 6, wherein the step for collecting the mixture of ethylene glycol and water running off from an airplane is acheived by collecting said mixture in an existing sewage collector;
and the step for carrying of said mixture in the first reservoir is achieved with a first piping having opposite ends, one end of said piping being connected to said sewage collector while the opposite end thereof is connected to the first reservoir, said first piping further comprising a pump.
8. A method according to claim 7, wherein admixing of lime with the mixture of ethylene glycol and water is achieved by bubbling of air with an air injector dipped in the first reservoir,
9. A method according to claim 7, wherein admixing of lime with the mixture of ethylene glycol and water is achieved with a propeller dipped in the first reservoir and driven in rotation by a motor.
10. A method according to claim 2, 3, 4, 5 or 6, wherein the step for collecting the lower phase of the first reservoir is acheived with a second piping having opposite ends, one end of said second piping being connected to the bottom of the first reservoir while the opposite end thereof is connected to the second reservoir, said second piping further comprising a pump.
11. A method according to claim 7, wherein the step for collecting the lower phase of the first reservoir is acheived with a second piping having opposite ends, one end of said second piping being connected to the bottom of the first reservoir while the opposite end thereof is connected to the second reservoir, said second piping further comprising a pump.
12. A method according to claim 2, 3, 4, 5 or 6, wherein the step for collecting the upper phase of the first reservoir is acheived with a third piping having opposite ends, one end of said third piping being connected to a portion of the first reservoir that is located above an interface slurry - ethylene glycol, while the opposite end thereof is connected to the third reservoir, said third piping further comprising a pump.
13. A method according to claim 11, wherein the step for collecting the upper phase of the first reservoir is acheived with a third piping having opposite ends, one end of said third piping being connected to a portion of the first reservoir that is located above an interface slurry - ethylene glycol, while the opposite end thereof is connected to the third reservoir, said third piping further comprising a pump.
14. A device for recovering glycol(s) from a mixture of glycol(s) and water, wherein it comprises:
- a first, a second and a third reservoirs;
- means for filling the first reservoir with a mixture of glycol(s) and water;
- means for introducing and admixing with the mixture of glycol(s) and water contained in the first reservoir, a sufficient amount of a compound intended to react with water of said mixture, give a product insoluble in water and form a slurry in which at least said insoluble product is suspended and in which glycol(s) are insoluble;
- means allowing the mixture of glycol(s) and slurry to separate into two distinct phases, that is an upper phase essentially consisting of glycol(s) and a lower phase essentially consisting of the above mentioned slurry;
- means for collecting and carrying the lower phase into the second reservoir;
- means for collecting and carrying the upper phase into the third reservoir.
15. A device for recovering ethylene glycol from a mixture of ethylene glycol and water obtained after having use ethylene glycol for de-icing an aircraft, said device comprising:
- a first, a second and a third reservoirs;
- means for collecting a mixture of ethylene glycol and water running off from an aircraft when ethylene glycol is applied against it to melt ice formed thereon;
- means for carrying said collected mixture of ethylene glycol and water, into the first reservoir;
- means for introducing and admixing with the mixture of ethylene glycol and water contained in the first reservoir, a sufficient amount of a compound intended to react with water of the mixture, give a product insoluble in water and form a slurry in which said insoluble product is suspended and in which ethylene glycol is insoluble;
- means allowing the mixture of ethylene glycol and slurry to separate into two distinct phases, that is an upper phase essentially consisting of ethylene glycol, and a lower phase essentially consisting of the above mentioned slurry;
- means for collecting and carrying the lower phase into the second reservoir;
- means for collecting and carrying the upper phase into the third reservoir.
16. A device according to claim 15, wherein means for collecting the mixture of ethylene glycol and water running off from an airplane consists of an existing sewage collector; and means for carrying said mixture in the first reservoir consist of a first piping having opposite ends, one end of said piping being connected to said sewage collector while the opposite end thereof is connected to the first reservoir, said first piping further comprising a pump.
17. A device according to claim 15, wherein means for introducing and admixing with the mixture ethylene glycol and water contained in the first reservoir a sufficient amount of a compound intended to react with water, obtain a product insoluble in water and form a slurry in which at least said insoluble product is suspended and in which ethylene glycol is insoluble, consist of a bin located above the first reservoir, communicating with an interior of the first reservoir and filled with said compound in powdered form, and of either an air injector dipped in the first reservoir and allowing a pressurized flow of air to bubble in the first reservoir or a propeller dipped in the first reservoir and driven by an electric motor, and means allowing the mixture of ethylene glycol and slurry to separate into two distinct phases consist of stopping the bubbling of air in the first reservoir or stopping the propeller in the first reservoir.
18. A device according to claim 17, wherein means for introducing and admixing with the mixture ethylene glycol and water contained in the first reservoir a sufficient amount of a compound intended to react with water, obtain a product insoluble in water and form a slurry in which at least said insoluble product is suspended and in which ethylene glycol is insoluble, consist of a bin located above the first reservoir, communicating with an interior of the first reservoir and filled with said compound in powdered form, and of either an air injector dipped in the first reservoir and allowing a pressurized flow of air to bubble in the first reservoir or a propeller dipped in the first reservoir and driven by an electric motor, and means allowing the mixture of ethylene glycol and slurry to separate into two distinct phases consist of stopping the bubbling of air in the first reservoir or stopping the propeller in the first reservoir.
19. A device according to claim 16, wherein means for collecting and carrying the lower phase in the second reservoir consist of a second piping having opposite ends, one end of said second piping being connected to the bottom of the first reservoir while the opposite end thereof is connected to the second reservoir, said second piping further comprising a pump.
20. A device according to claim 18, wherein means for collecting and carrying the lower phase in the second reservoir consist of a second piping having opposite ends, one end of said second piping being connected to the bottom of the first reservoir while the opposite end thereof is connected to the second reservoir, said second piping further comprising a pump.
21. A device according to claim 16, wherein means for collecting and carrying the upper phase in the third reservoir consist of a third piping having opposite ends, one end of said third piping being connected to a portion of the first reservoir that is located above an interface slurry - ethylene glycol, while the opposite end thereof is connected to the third reservoir, said third piping further comprising a pump.
22. A device according to claim 20, wherein means for collecting and carrying the upper phase in the third reservoir consist of a third piping having opposite ends, one end of said third piping being connected to a portion of the first reservoir that is located above an interface slurry - ethylene glycol, while the opposite end thereof is connected to the third reservoir, said third piping further comprising a pump.
23. A device according to claim 16, wherein the second and third reservoirs are each further provided with means allowing to recover their content.
24. A device according to claim 16, wherein the second reservoir is further provided with a fourth piping having opposite ends, one end of said fourth piping being connected with the bottom of the second reservoir while the opposite end thereof is connected to a valve, said fourth piping further comprising a pump.
25. A device according to claim 22, wherein the second reservoir is further provided with a fourth piping having opposite ends, one end of said fourth piping being connected with the bottom of the second reservoir while the opposite end thereof is connected to a valve, said fourth piping further comprising a pump.
26. A device according to claim 16, wherein the third reservoir is further provided with a fifth piping having opposite ends, one end of said fifth piping being connected with the bottom of the third reservoir while the opposite end thereof is connected to a valve, said fifth piping further comprising a pump.
27. A device according to claim 24, wherein the third reservoir is further provided with a fifth piping having opposite ends, one end of said fifth piping being connected with the bottom of the third reservoir while the opposite end thereof is connected to a valve, said fifth piping further comprising a pump.
CA002074031A 1992-07-16 1992-07-16 Method and device for recovering glycol(s) from a mixture of glycol(s) and water Abandoned CA2074031A1 (en)

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CA002074031A CA2074031A1 (en) 1992-07-16 1992-07-16 Method and device for recovering glycol(s) from a mixture of glycol(s) and water

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CA002074031A CA2074031A1 (en) 1992-07-16 1992-07-16 Method and device for recovering glycol(s) from a mixture of glycol(s) and water

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5928477A (en) * 1998-01-07 1999-07-27 Inland Technologies Inc. Method and apparatus for removing water from an aqueous fluid mixture

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5928477A (en) * 1998-01-07 1999-07-27 Inland Technologies Inc. Method and apparatus for removing water from an aqueous fluid mixture

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