EP3621921A1 - Concentrated aqueous solutions of aluminum chlorohydrate monohydrate - Google Patents
Concentrated aqueous solutions of aluminum chlorohydrate monohydrateInfo
- Publication number
- EP3621921A1 EP3621921A1 EP18731244.2A EP18731244A EP3621921A1 EP 3621921 A1 EP3621921 A1 EP 3621921A1 EP 18731244 A EP18731244 A EP 18731244A EP 3621921 A1 EP3621921 A1 EP 3621921A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- solution
- aluminum chlorohydrate
- water
- less
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- -1 aluminum chlorohydrate monohydrate Chemical compound 0.000 title claims abstract description 37
- 239000007864 aqueous solution Substances 0.000 title description 2
- LVYZJEPLMYTTGH-UHFFFAOYSA-H dialuminum chloride pentahydroxide dihydrate Chemical compound [Cl-].[Al+3].[OH-].[OH-].[Al+3].[OH-].[OH-].[OH-].O.O LVYZJEPLMYTTGH-UHFFFAOYSA-H 0.000 claims abstract description 74
- 239000000843 powder Substances 0.000 claims abstract description 73
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 41
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052742 iron Inorganic materials 0.000 claims abstract description 17
- 238000007710 freezing Methods 0.000 claims abstract description 14
- 230000008014 freezing Effects 0.000 claims abstract description 14
- 239000008236 heating water Substances 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- CVAGXMIIJWVUAF-UHFFFAOYSA-N hypochlorous acid;hydrate Chemical compound O.ClO CVAGXMIIJWVUAF-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 157
- 239000006185 dispersion Substances 0.000 description 12
- 238000009736 wetting Methods 0.000 description 12
- 239000007787 solid Substances 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 6
- 239000000701 coagulant Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- 239000000428 dust Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 150000004687 hexahydrates Chemical class 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004682 monohydrates Chemical class 0.000 description 1
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
- C01F7/57—Basic aluminium chlorides, e.g. polyaluminium chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
- C01P2006/33—Phase transition temperatures
- C01P2006/34—Melting temperatures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Definitions
- the present invention is directed to aluminum chlorohydrate products, and more particularly, to systems and processes for producing aluminum chlorohydrate products for use in the treatment of water and/or wastewater.
- ACH aluminum chlorohydrate
- hydrochloric acid aluminum chloride or basic aluminum chloride solutions.
- the aluminum metal typically contains up to 0.2 wt% iron.
- the iron acts like a catalyst and speeds up the reaction to form the ACH solution.
- the process produces ACH solutions of greater than 150 ppm as Fe. If a lower iron content is desired, extra processing steps are required to remove the iron from the ACH solution.
- ACHDH 50% aluminum chlorohydrate dihydrate
- this product requires additional heating to keep from freezing in much of the country if stored outdoors during winter.
- These solutions are often spray dried to produce ACHDH in a solid, powder form.
- ACHDH is readily soluble in cold water and can be easily diluted with water to produce the 50% ACHDH solution.
- these products have problems working as a flocculent during cold water conditions and in certain circumstances do not work in a very efficient manner.
- Powder wetting and dispersion systems are common for putting powders into solution. However, when these systems are used to put aluminum chlorohydrate monohydrate into solution using conventional methods, the system becomes filled with gel solids and ceases to operate.
- the method further includes dissolving another portion of the aluminum chlorohydrate monohydrate powder into the solution.
- Dissolving may include agitating the aluminum chlorohydrate monohydrate powder and the heated water until the solution is clear.
- the method may further include mixing the solution of aluminum
- Heating the second solution to at least 150°F and less than 200°F may include heating the second amount of water to a temperature sufficiently above 150°F, so that adding the heated second amount of water to the solution of aluminum chlorohydrate causes the temperature of the second solution to be at least 150°F and less than 200°F.
- the first solution or the second solution may include an aluminum oxide concentration greater than 24 wt % and less than 27 wt % or greater than 18 wt % and less than 27 wt %.
- the second solution may have a basicity greater than 74% and less than 83%.
- the solution may have a freezing point ranging from about 10°F to about 16 °F.
- the solution may have an iron content of less than 70 ppm as Fe. Products produced by these methods are also disclosed.
- the aluminum oxide concentration in the solution may range from about 24 wt % to about 27 wt %.
- the solution may have an iron content of between about 0 to about 70 ppm as Fe.
- a mixing system for forming a solution of aluminum chlorohydrate according to the above methods is also provided.
- FIG. 1 is a graph of the turbidity vs. amount of coagulant for a prior art aluminum chlorohydrate solution and solution made according to Example 7;
- FIG. 2 is a graph of the ultraviolet light absorption vs. amount of coagulant for a prior art aluminum chlorohydrate solution and solution made according to Example 7;
- FIG. 3 is a graph of the turbidity vs. amount of coagulant for a prior art aluminum chlorohydrate solution and solution made according to Example 7;
- FIG. 4 is a graph of the turbidity vs. amount of coagulant for a prior art aluminum chlorohydrate solution and solution made according to Example 8;
- FIG. 5 is a graph of a nuclear magnetic resonance (NMR) spectrum for a powder used to make the Example 7 solution according to embodiments of the present invention.
- FIGS. 6 and 7 are graphs of NMR spectrums for prior art aluminum chlorohydrate powders
- FIG. 8 shows a process of forming a solution of aluminum chlorohydrate from aluminum chlorohydrate monohydrate powder according to embodiments of the present invention.
- FIG. 9 schematically shows a mixing system for forming a solution of aluminum chlorohydrate from aluminum chlorohydrate monohydrate powder according to embodiments of the present invention.
- Percent Basicity is defined as (%OH)(52.91)/(% Al). On a molar level, this may be expressed as ((OH)/(Al))/3 multiplied by 100. Thus, Al 2 (OH) 2 Cl 4 has a basicity of 33%.
- UV 254" is absorption of ultraviolet light at 254 nm though a 10 cm cuvette of water.
- Powder wetting and dispersion systems are commercially available systems that are specifically designed to wet and disperse powders into liquids. Most powder wetting and dispersion systems use induction created by a mixer or pump to suck the powder into the liquid and then shear the mixture to assure uniformity.
- a system and method for producing an aluminum chlorohydrate solution from aluminum chlorohydrate monohydrate (ACHMH) powder are described herein according to embodiments of the present invention.
- ACHMH powder produced by decomposing aluminum chloride is described herein according to embodiments of the present invention.
- ACHDH commercially available aluminum chlorohydrate dihydrate
- ACHMH powder may be produced as described in U.S. Pat. Appl. Publ. No. 2016/0074873, which is incorporated by reference herein in its entirety. These ACHMH powders are mostly insoluble in cold water and solutions produced from these ACHMH powders are more efficient as flocculants than commercially available ACH solutions produced by prior art methods. Embodiments of the present invention produce solutions from these ACHMH powders that have a higher chloride content and hence a lower freezing point, and tend to require a somewhat lower basicity than similar solutions produced using ACHDH powder. The ACHMH powders are more economical to produce than the prior art since the process does not require expensive aluminum metal to produce the
- ACHMH product ACHMH product.
- the ACHMH powder weighs less than the produced solution and hence can be more economical than liquid to ship.
- the powdered ACHMH product can be described as
- ACHMH powders are different from ACHDH in that they have significant pentahedral structures when compared to ACH produced by a prior art metal process. The differences can be seen by comparing FIG. 5 to FIGS. 6 and 7. These pentahedral species are more efficient than commercial ACH products at removing impurities from water during flocculation. For example, the solutions of these powders remove more turbidity and organics as measured by UV-254, as shown in FIGS. 1-4. Tables 1-4 (shown below) show the data plotted in FIGS. 1-4, respectively. Solutions of these ACHMH powders can be formulated so that they tolerate freezing temperatures better than conventional, prior art ACH solutions. In addition, since iron is not needed as a catalyst for the processes of making the ACHMH powder, commercially available lower iron raw materials can be used. Without any additional processing, the iron content of the solution will be less than 70 ppm as Fe.
- FIG. 8 shows a process 100 for forming a lower basicity aluminum chlorohydrate solution from the ACHMH powders according to embodiments of the present invention.
- the process 100 begins by providing an ACHMH powder having a composition of:
- step 120 water is heated to at least about 120°F and less than about 200°F.
- the problem of putting a large volume of ACHMH powder into a small amount of liquid can be solved by starting with a base of ACH solution. As much or as little as practical may be used. For example, approximately 25% starting material may provide an adequate solution for solubilizing without an additional large capital expense for extra tankage.
- the ACH solution should be heated with all the water to above 150°F to make the solution according to embodiments of the present invention. If desired, the water can be heated above 150°F and added to the cooler ACH solution to allow the use of more economical materials of construction. Heat exchangers that can tolerate the corrosiveness of ACH are made of exotic metals or silicon carbide and are more expensive than those that simply heat water.
- step 130 the ACHMH powder is added to the heated solution and allowed to agitate until clear.
- the process of putting the ACHMH powder in solution is exothermic and may raise the temperature of the mixing tank up to 180°F or above depending on the starting temperature of the solution.
- the ACHMH powder may be added in stages to prevent gelation. Up to half of the Aluminum chlorohydrate monohydrate (ACHMH) is added to all the water at above 120°F and allowed to completely dissolve. The rest is added at several equal increments after each increment is incorporated. This process may take approximately 1 hour.
- ACHMH Aluminum chlorohydrate monohydrate
- FIG. 9 shows a mixing system 10, formed using a powder wetting and dispersion system, to form the aluminum chlorohydrate solution according to the process of FIG. 8.
- the mixing system 10 may include an agitated tank or mixing tank 12 for holding and mixing the liquids used and produced in the mixing system 10.
- the mixing tank 12 may be initially loaded with ambient temperature water and then the water may be circulated, using circulator pump 14, along path 16 and path 18, through a heat exchanger 20 that heats the water to at least about 150°F and less than the boiling temperature of the liquid, e.g., less than about 200°F.
- steam 22 may be an input to the heat exchanger 20 and condensate 24 may be removed from the heat exchanger 20.
- the heated water then returns along path 26 to the mixing tank 12.
- the water may be circulated in the mixing system 10 in this manner until all of the water in the mixing tank 12 has been heated to the desired temperature.
- the heated water may then be circulated along path 28, through an optional heat exchanger 30 that cools, and then introduced into a powder wetting and dispersion system 40.
- the heat exchanger 30 may include a cooling water supply 32 as an input and a cooling water return 34 as an output.
- the heat exchanger 30 may be set with an exit temperature of ambient to about 140°F, preferably between about 120°F and about 130°F.
- the ACHMH powder may be held in a hopper 36 and gradually added to the powder wetting and dispersion system 40 along with the heated water to form a solution of aluminum chlorohydrate.
- the aluminum chlorohydrate solution is then returned back to the mixing tank 12 along path 42 where the aluminum chlorohydrate solution is mixed with the heated water.
- the heated solution is then circulated back through path 16 and path 28, through the heat exchanger 30 to the powder wetting and dispersion system 40 to be combined with the ACHMH powder and then the aluminum chlorohydrate solution is returned to the mixing tank 12 along path 42.
- Some of the heated solution from the mixing tank 12 may be circulated back along path 18 through the heat exchanger 20, along path 26 and back to the mixing tank 12 in order to keep the aluminum chlorohydrate solution at a desired temperature.
- the process continues until all the ACHMH powder is dispensed from the hopper 36 and added into the aluminum chlorohydrate solution.
- the aluminum chlorohydrate solution may then continue to circulate along path 16 and path 18, through heat exchanger 20, along path 26 and back to mixing tank 12 until the aluminum chlorohydrate solution is heated to at least about 150 °F and less than about 200°F and forms a clear solution.
- the aluminum chlorohydrate solution may then be feed along path 44 and collected in a storage tank 46 for further use.
- Example 4 Unsuccessful effort at putting ACH monohydrate into solution at 176 °F
- 24 grams of aluminum chlorohydrate monohydrate at 56.6% A1 2 0 3 and 83% basic was added to a beaker containing 35 milliliters of water at 176 °F. The mixture became a solid mass, creating an unusable product.
- Example 7 Successful effort at putting ACH monohydrate into solution according to embodiments of the present invention
- FIGS. 1-3 are graphs showing the turbidity and ultraviolet light absorption versus the amount of coagulant for the solution made according to Example 7 compared to the prior art. Tables 1-3 below show the data for FIGS. 1-3, respectively.
- the ACH powder is very dusty so that an induction line was used to vacuum the product into the tank.
- the tank was also equipped with a stack that contained water spray nozzles to prevent dust from spreading.
- the mixture was agitated for about an hour until a clear solution was obtained.
- This also produced a clear solution after filtration producing a solution of 25% A1 2 0 and 79% basicity.
- the solution had a freezing point of 12°F and an iron content of 32 ppm as Fe.
- the solution remained nonviscous and usable for over a year.
- FIG. 4 is a graph showing the turbidity versus the amount of coagulant for the solution made according to Example 8 compared to the prior art. Table 4 below shows the data for FIG. 4.
- Example 9 Successful effort at putting ACH monohydrate into solution according to embodiments of the present invention
- Example 10 Successful effort at putting ACH monohydrate into solution according to embodiments of the present invention
- the solution remained nonviscous and clear for over a year.
- the solution had a freezing point of 22°F and an iron content as Fe of 29 ppm.
- Example 11 Successful effort at putting ACH monohydrate into solution according to embodiments of the present invention
- Example 10 In order to produce a 26.5% aluminum oxide solution, 50 grams of Example 10 at 178°F was added to a beaker. To the beaker was added 36 milliliters of water at 210°F. This solution had a temperature of 190°F. To this solution was added 50 grams of ACHMH at 46.6% A1 2 0 3 and 73.8% basic, having the formula of:
- Jar Testing was performed comparing ACH produced by the standard commercial metal digesting process versus the ACH solution produced according to embodiments of the present invention by solutionizing ACHMH powder. The testing was done on raw waters from two municipalities in TN and KY using their respective jar testing techniques. The below results demonstrate better turbidity removal at the equivalent aluminum dosing for the ACH solution produced according to embodiments of the present invention.
- Example 14 Successful effort at putting ACH monohydrate into solution using a powder wetting and dispersion system according to embodiments of the present invention
- Example 7 The valve to the hopper was partially opened to allow the powder to gradually mix into the heated solution. The powder was allowed to flow at about 20 pounds per minute. After about 4 hours the addition was complete. The solution was allowed to continue through the heating heat exchanger until the temperature was 165°F. This produced 860 gallons of a clear nonviscous solution of 25% A1 2 0 and 79.1% basic.
Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201762505724P | 2017-05-12 | 2017-05-12 | |
US201762550303P | 2017-08-25 | 2017-08-25 | |
PCT/US2018/032276 WO2018209204A1 (en) | 2017-05-12 | 2018-05-11 | Concentrated aqueous solutions of aluminum chlorohydrate monohydrate |
Publications (1)
Publication Number | Publication Date |
---|---|
EP3621921A1 true EP3621921A1 (en) | 2020-03-18 |
Family
ID=62599685
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP18731244.2A Pending EP3621921A1 (en) | 2017-05-12 | 2018-05-11 | Concentrated aqueous solutions of aluminum chlorohydrate monohydrate |
Country Status (5)
Country | Link |
---|---|
EP (1) | EP3621921A1 (en) |
BR (1) | BR112019023284A2 (en) |
CA (1) | CA3062428A1 (en) |
MX (1) | MX2019013369A (en) |
WO (1) | WO2018209204A1 (en) |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1568831A (en) * | 1976-01-14 | 1980-06-04 | Unilever Ltd | Inhibition of perspiration |
US7846318B2 (en) * | 2006-01-06 | 2010-12-07 | Nextchem, Llc | Polyaluminum chloride and aluminum chlorohydrate, processes and compositions: high-basicity and ultra high-basicity products |
ES2843264T3 (en) | 2014-09-12 | 2021-07-16 | Usalco Llc | Production method of aluminum chloride derivatives |
-
2018
- 2018-05-11 MX MX2019013369A patent/MX2019013369A/en unknown
- 2018-05-11 BR BR112019023284A patent/BR112019023284A2/en active Search and Examination
- 2018-05-11 EP EP18731244.2A patent/EP3621921A1/en active Pending
- 2018-05-11 WO PCT/US2018/032276 patent/WO2018209204A1/en active Application Filing
- 2018-05-11 CA CA3062428A patent/CA3062428A1/en active Pending
Also Published As
Publication number | Publication date |
---|---|
CA3062428A1 (en) | 2018-11-15 |
BR112019023284A2 (en) | 2020-05-19 |
WO2018209204A1 (en) | 2018-11-15 |
MX2019013369A (en) | 2020-01-13 |
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