US3034985A - Amine flotation reagent preparation - Google Patents
Amine flotation reagent preparation Download PDFInfo
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- US3034985A US3034985A US136740A US13674061A US3034985A US 3034985 A US3034985 A US 3034985A US 136740 A US136740 A US 136740A US 13674061 A US13674061 A US 13674061A US 3034985 A US3034985 A US 3034985A
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- amine
- flotation
- acid
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- 150000001412 amines Chemical class 0.000 title claims description 69
- 239000003153 chemical reaction reagent Substances 0.000 title claims description 47
- 238000005188 flotation Methods 0.000 title claims description 39
- 238000002360 preparation method Methods 0.000 title description 7
- 239000000203 mixture Substances 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000002253 acid Substances 0.000 claims description 29
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 18
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- 150000003839 salts Chemical class 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-PWCQTSIFSA-N Tritiated water Chemical compound [3H]O[3H] XLYOFNOQVPJJNP-PWCQTSIFSA-N 0.000 claims 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 37
- -1 amine salt Chemical class 0.000 description 34
- 238000000034 method Methods 0.000 description 27
- 239000000243 solution Substances 0.000 description 26
- 239000000839 emulsion Substances 0.000 description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 13
- 238000000926 separation method Methods 0.000 description 11
- 238000006386 neutralization reaction Methods 0.000 description 10
- 150000007513 acids Chemical class 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 6
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 239000012266 salt solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 239000003760 tallow Substances 0.000 description 3
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 159000000021 acetate salts Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical class Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000000266 injurious effect Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000010698 whale oil Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/01—Organic compounds containing nitrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; Specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
- B03D2203/10—Potassium ores
Definitions
- Aliphatic amines have been used as a collector reagent for many different types of materials, and one important use of aliphatic amines has been in the flotation separation of sylvite from sylvinite ores.
- the aliphatic amines are generally utilized as a liquid preparation, which is added to an ore pulp with conditioning or mixingprior to the flotation treatment. In some cases considerable difficulty has been experienced in the preparation of the fluid reagent composition, and in a number of cases the liquid amine reagent composition has proved to be ineifectual to promote flotation separations.
- the commonly used aliphatic amines themselves are practically insoluble in water, and in order to prepare a liquid composition it has been the general practice to utilize the soluble salts of the amines with certain acids.
- the acetate salts of the aliphatic amines are widely used because of their more favorable solubility.
- the commercially available aliphatic amine reagents, which are in the form of their amineacetate salts, are dissolved in water at the flotation site.
- acetate salts of relatively high molecular weight aliphatic amines are used, and particularly the octadecyl, hexadecyl and oleyl amines and mixtures of these amines have been widely used.
- the actual hydrocarbon content of the commercial. amine salts depends on the source which the amines are manufactured.
- the aliphatic amines which have found general use are those prepared from such materials such as tallow, lard, soybean oil, whale oil, coconut oil and other common oils and fats. -Some of the products may be hydrogenated to reduce unsaturation and thus produce materials of higher melting points.
- the method of preparation of the amine acetate which is accomplished by adding acetic acid to the amine, in many instances causes chemical changes in the compounds reducing their elfectiveness as collector reagents.
- the composition On adding acetic acid to the amine, the composition is heated by the exothermic reaction. Often hot spots occur in the batch due to inadequate mixing and the amine in the local hot zone is converted into a substance that actually injures flotation.
- the amine acetate when the amine acetate ism-aintained at an elevated temperature, even when the temperature is not high enough to cause instantaneous injury, for a substantial period of time, the amine ucef merse the amine acetate in its shipping barrel, the standand container for shipping the amine acetate, in hot water to melt the amine and allow it to escape from the barrel. If the amine acetate is heated without melting and escaping into the water and it is maintained in that stage for a substantial length of time, the deleterious conversion occurs.
- the process of the invention provides a means for producing an amine salt solution simply and economically, and provides means for producing either a true solution of the amine salt or an emulsion of the amine in an amine salt solution.
- the process of the invention comprising melting a minor amount of an aliphatic amine in a major portion of water, and after the amine is completely melted, an amount of acid is added to the resultant fluid to convert at least a portion of the amine into a water soluble salt.
- acid as acetic, nitric, hydrochloric, formic, hydrobromic, etc. produce salts of sufiicient solubility as to form effective reagent solutions or emulsions.
- a stoichiometric amount of acid is added to the amine and Water liquor to convert substantially all of the aliphatic amine.
- a lesser amount of acid is introduced into the amine liquor to convert less than the total amount of the amineto thereby produce an emulsion of the amine in an amine salt solution.
- Solutions of amine salts are very effective reagents in concentrations of 2% and the emulsions of the partially neutralized amines have been found to be highly effective reagents as 25% emulsions.
- EXAMPLE I A 2% by weight aqueous solution of an aliphatic amine acetate flotation reagent solution may be obtained I EXAMPLE II
- a. hydrogenated tallow amine By using the directions of Example I, and by using a. hydrogenated tallow amine, a very viscous liquor is produced on heating the same quantity. of water and hydrogenated tallow amine. The viscous solution is very difiicult to handle.
- the mixture becomes a creamy emulsion and on cooling aosasae it remains liquefied and readily handled. In this case the amine is only partially neutralized (about 34%), so an emulsion of the hydrogenated tallow amine is produced in a hydrogenated tallow amine acetate solution.
- Partial neutralization provides substantial advantages in that it produces greater concentrations of the reagent as an emulsion rather than as a true solution.
- concentrations of the reagent as an emulsion rather than as a true solution.
- by neutralizing about 30% based on an equivalent of the amine Very stable emulsions are produced.
- the emulsions of tallow amine may be made in concentrations as much as about 5% or slightly above, at ambient or room temperature, while true solutions are essentially l mited to around 2% or less, depending upon the particular salt.
- stoichiometric neutralization is desirable so as to produce an emulsion.
- the partially neutralized compositions are, in effect, colloidal solutions. These reagents as partially ncutralized colloidal solutions are very easy to handle at room temperature. They are, also, very efiective as flotation reagents in the lower to the higher concentrations.
- the salts and colloidal solutions of other acids were prepared by following either the procedure of Example I for 100% neutralization, or by the procedure of Example 11 to produce the 30% neutralization which forms the emulsions or colloidal solutions.
- EXAMPLE nr Following the procedure of Example II, about 200 pounds of hydrogenated tallow amine was treated with about 70.5 pounds of 37.5% hydrochloric acid, which gave a 100% neutralization of the tallow amine, which is based on a molecular combined Weight of 275. This neutralization was performed by adding the acid to the amine, which had been melted in about 9756 pounds of water. A 30% neutralization is produced by reacting about 21.2 pounds of 37.5% hydrochloric acid with the 200 pounds of amine previously melted in an equivalent amount of water. Both reagents showed very good activity as flotation reagents. In addition, the solutions handled easily and stored very well.
- solubility of the resulting amine salt seems to be the determining factor for choice of the precursor acid for the neutralization. Acids which produce amine salts of essentially no water solubility do not form useful emulsions and obviously do not form true aqueous solutions. The stability of the emulsion of the amine also is a factor, since an unstable emulsion would not produce the desired flotation results.
- the acetic acid and hydrochloric acid produce excellent salts for flotation reagents both as true solutions and preferably as emulsions.
- the nitric, formic and hydrobromic acids also produce good solutions or emulsions since the amine salt of each has good solubility.
- the invention has been specifically illustrated by certain examples, it is applicable to the full range of aliphatic amines normally used in flotation.
- other acids maybe utilized to form other acid salts of the amine in solution
- the acetate, hydrochloride are the preferred acids since these compositions have generally favorable solubility characteristics.
- the amine reagents are normally used in low percentage solutions or emulsions (on the order of one-half to five percent), it is preferable to maintain the volume of water sufficiently high to initially produce the low percent solutions without adding more water. It has been found satisfactory, however, to prepare concentrated solutions and then add water to such a concentrated solution prior to the use of the solution as a flotation reagent.
- the concentrated amine produced by either com.- position methods are easily stored and are not subject to deterioration.
- a process for preparing a liquefied amine collector reagent for flotation separations the steps of melting a minor quantity of a normally solid, high molecular weight aliphatic amine composition in a major quantity of water, and then introducing into the resultant liquor a sufiicient amount of an acid to react with not more than a stoichiometric amount of the amine present in the liquor, and forming therewith a water soluble salt of the amine whereby to form a stabilized aqueous amine composition containing at least about 1% by weight of the amine composition.
- a process for preparing a liquefied amine collector reagent for flotation separations the steps of melting a minor quantity of a normally solid, high molecular weight aliphatic amine composition in a major quantity of water, and then introducing into the resultant liquor a sufiicient amount of an acid to react with not more than a stoichiometric amount of the amine present in the liquor, and forming therewith a water soluble salt of the amine whereby to form a stabilized aqueous amine composition containing from about 1-5% by weight of the amine composition.
- a process for preparing a liquefied amine collector reagent for flotation separations the steps of melting a minor quantity of a normally solid, high molecular weight aliphatic amine composition in a major quantity of water, and then introducing into the resultant liquor a stoichiometric amount of an acid which'reacts with the amine present in the liquor to form a soluble salt thereof, whereby to form an aqueous stabilized amine salt solution.
- a process for preparing a liquefied amine collector reagent for flotation separations the steps of melting a minor quantity of a normally solid, high molecular weight aliphatic amine composition in a major quantity of water, and then introducing into the resultant liquor about 30% of a stoichiometric amount of acetic acid which reacts with the amine present in the liquor to form a soluble amine acetate salt, and thereby form an aqueous, stabilized amine composition containing at least about 1% of the amine composition by weight.
- a process for preparing a liquefied amine collector reagent for flotation separations the steps of melting a minor quantity of a normally solid, high molecular weight aliphatic amine composition in a major quantity of water, and then introducing into the resultant liquor about 30% of a stoichiometric amount of hydrochloric acid which reacts with the amine present in the liquor to form a soluble amine chloride salt thereof, and thereby form m aqueous stabilized amine composition containing at. least about 1% of the amine composition by weight.
- a process of preparing a liquefied amine collector reagent for flotation separations the steps of melting not more than about 5% by weight of an aliphatic amine composition in at least about by weight of water, and then introducing into the resultant liquor substantially less than a stoichiometric amount of acetic acid to react with a portion of the liquefied amine whereby to form a stabilized emulsion of the aliphatic amine in an aliphatic amine acetate-water solution.
Landscapes
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Description
3,tl3 t,9tl5 AMHNIE FLUTATHUN REAGENT PRERARATKGN Edmund A. Schoeltl, tCarlsbad, N. Men, assignor to yotash Company of America, Carlsbad, N. Mex., a corporation of Golorado No Drawing. lFilcd Sept. 8, 1961, Ser. No. 1$6,74-il 2d illaims. (ill. Mil-61) This invention relates to improvements in the flotation art, and more particularly it relates to a process for preparing amine salt flotation reagents, and this application is a continuation-in-partof my copending application Serial No. 707,863, filed January 9, 1958, now abandoned, for Amine Flotation Reagent Preparation.
Aliphatic amines have been used as a collector reagent for many different types of materials, and one important use of aliphatic amines has been in the flotation separation of sylvite from sylvinite ores. The aliphatic amines are generally utilized as a liquid preparation, which is added to an ore pulp with conditioning or mixingprior to the flotation treatment. In some cases considerable difficulty has been experienced in the preparation of the fluid reagent composition, and in a number of cases the liquid amine reagent composition has proved to be ineifectual to promote flotation separations.
The commonly used aliphatic amines themselves are practically insoluble in water, and in order to prepare a liquid composition it has been the general practice to utilize the soluble salts of the amines with certain acids. For this purpose, the acetate salts of the aliphatic amines are widely used because of their more favorable solubility. The commercially available aliphatic amine reagents, which are in the form of their amineacetate salts, are dissolved in water at the flotation site.
For a general flotation reagent, acetate salts of relatively high molecular weight aliphatic amines are used, and particularly the octadecyl, hexadecyl and oleyl amines and mixtures of these amines have been widely used. The actual hydrocarbon content of the commercial. amine salts depends on the source which the amines are manufactured. The aliphatic amines which have found general use are those prepared from such materials such as tallow, lard, soybean oil, whale oil, coconut oil and other common oils and fats. -Some of the products may be hydrogenated to reduce unsaturation and thus produce materials of higher melting points.
Commercially available aliphatic amine acetates are purchased as such, and are placed in hot water to melt and dissolve the same at the site of use. This preparation of these reagent compositions has resulted in variable flotation results, and in fact some batches of the reagent have been found to be ineffectual for flotation. Where flotation problems are the result of the amine reagent itself, it is very diflicult to trace the trouble. This is especially true when ditferent portions of a batch or a barrel of the aliphatic amine acetate gives ditferent flotation results. Due to the ditliculty of tracing the trouble caused by a poor amine reagent, often the reagent is used up before the cause of the poor flotation results can be recognized as being in the particular reagent batch.
The method of preparation of the amine acetate, which is accomplished by adding acetic acid to the amine, in many instances causes chemical changes in the compounds reducing their elfectiveness as collector reagents. On adding acetic acid to the amine, the composition is heated by the exothermic reaction. Often hot spots occur in the batch due to inadequate mixing and the amine in the local hot zone is converted into a substance that actually injures flotation. Also, when the amine acetate ism-aintained at an elevated temperature, even when the temperature is not high enough to cause instantaneous injury, for a substantial period of time, the amine ucef merse the amine acetate in its shipping barrel, the standand container for shipping the amine acetate, in hot water to melt the amine and allow it to escape from the barrel. If the amine acetate is heated without melting and escaping into the water and it is maintained in that stage for a substantial length of time, the deleterious conversion occurs.
It has been found that once an aqueous solution has been made of the amine' acetate, no further conversion occurs, since the conversion consists generally of a dehydration. Thus once an aqueous solution of relatively low content of amine acetate is achieved, the amine acetate reagent is relatively free from further conversion.
Included among the objects and advantages of the present invention is to provide aprocess for preparing an amine solution Without converting part or all of the amine salt to a material that is ineffectual or injurious to a'flotation separation. The process of the invention provides a means for producing an amine salt solution simply and economically, and provides means for producing either a true solution of the amine salt or an emulsion of the amine in an amine salt solution. The process, further, I
provides a means for producing uniformly standard amine salt flotation reagent liquids which may be stored for considerable periods of time Without deteriorating.
In general, the process of the inventioncomprising melting a minor amount of an aliphatic amine in a major portion of water, and after the amine is completely melted, an amount of acid is added to the resultant fluid to convert at least a portion of the amine into a water soluble salt. Such acids as acetic, nitric, hydrochloric, formic, hydrobromic, etc. produce salts of sufiicient solubility as to form effective reagent solutions or emulsions. In one form of the invention, a stoichiometric amount of acid is added to the amine and Water liquor to convert substantially all of the aliphatic amine. In another modification', a lesser amount of acid is introduced into the amine liquor to convert less than the total amount of the amineto thereby produce an emulsion of the amine in an amine salt solution. Solutions of amine salts are very effective reagents in concentrations of 2% and the emulsions of the partially neutralized amines have been found to be highly effective reagents as 25% emulsions.
in carrying out the objects and advantages of the invention, the following examples illustrate a preparation I of several reagent compositions:
EXAMPLE I A 2% by weight aqueous solution of an aliphatic amine acetate flotation reagent solution may be obtained I EXAMPLE II By using the directions of Example I, and by using a. hydrogenated tallow amine, a very viscous liquor is produced on heating the same quantity. of water and hydrogenated tallow amine. The viscous solution is very difiicult to handle. By adding 13 pounds of acetic acid, the mixture becomes a creamy emulsion and on cooling aosasae it remains liquefied and readily handled. In this case the amine is only partially neutralized (about 34%), so an emulsion of the hydrogenated tallow amine is produced in a hydrogenated tallow amine acetate solution.
Under normal conditions, hydrogenated tallow amine acetate has such a low solubility that in prior practices it was found necessary to maintain the mixture hot to insure satisfactory feeding as a flotation reagent. However, by using the procedure of the present invention which includes melting the amine in water and then adding the acetic acid, the quantity of the acetic acid may be adjusted so as to secure a readily handled emulsion. Such an emulsion, also retains its easy handling characteristics when cooled.
Partial neutralization, as set forth in Example II, provides substantial advantages in that it produces greater concentrations of the reagent as an emulsion rather than as a true solution. As provided in the example, by neutralizing about 30% based on an equivalent of the amine, Very stable emulsions are produced. The emulsions of tallow amine may be made in concentrations as much as about 5% or slightly above, at ambient or room temperature, while true solutions are essentially l mited to around 2% or less, depending upon the particular salt. Thus, where higher concentrations of the reagent are desired in a flotation process, less than stoichiometric neutralization is desirable so as to produce an emulsion. It has been found that at about neutralization of an equivalent of the amine produces a very stable emulsion at generally higher concentrations of reagent in the aqueous 30 mixture. After preparing the reagent aqueous compositions, the reagents were used in actual flotation tests to determine the characteristics of the reagent.
The partially neutralized compositions are, in effect, colloidal solutions. These reagents as partially ncutralized colloidal solutions are very easy to handle at room temperature. They are, also, very efiective as flotation reagents in the lower to the higher concentrations.
The salts and colloidal solutions of other acids were prepared by following either the procedure of Example I for 100% neutralization, or by the procedure of Example 11 to produce the 30% neutralization which forms the emulsions or colloidal solutions.
EXAMPLE nr Following the procedure of Example II, about 200 pounds of hydrogenated tallow amine was treated with about 70.5 pounds of 37.5% hydrochloric acid, which gave a 100% neutralization of the tallow amine, which is based on a molecular combined Weight of 275. This neutralization was performed by adding the acid to the amine, which had been melted in about 9756 pounds of water. A 30% neutralization is produced by reacting about 21.2 pounds of 37.5% hydrochloric acid with the 200 pounds of amine previously melted in an equivalent amount of water. Both reagents showed very good activity as flotation reagents. In addition, the solutions handled easily and stored very well.
In the following of the procedure above, solutions and compositions of the amine with other acids were prepared, and the results tabulated in the following table:
Acid Required to Neutralize 200 Lbs. of Amine (Mal. Comb. Wt. of 275) to and 30% Levels 0f the salts set forth in the table above, the nitrate, yr;
4, formats and bromide amine salts produced good emulsions which performed very well in flotation tests. The amine phosphate produced from orthophosphoric acid is based on 1% hydrogens entering the neutralization step, but the amine phosphate is of limited solubility and are not desirable for normal flotation procedures. Similarly, the amine sulfate is of low solubility and its usefulness as a flotation reagent is quite limited.
The solubility of the resulting amine salt seems to be the determining factor for choice of the precursor acid for the neutralization. Acids which produce amine salts of essentially no water solubility do not form useful emulsions and obviously do not form true aqueous solutions. The stability of the emulsion of the amine also is a factor, since an unstable emulsion would not produce the desired flotation results.
The acetic acid and hydrochloric acid produce excellent salts for flotation reagents both as true solutions and preferably as emulsions. The nitric, formic and hydrobromic acids also produce good solutions or emulsions since the amine salt of each has good solubility.
While the invention has been specifically illustrated by certain examples, it is applicable to the full range of aliphatic amines normally used in flotation. Also, while other acids maybe utilized to form other acid salts of the amine in solution, the acetate, hydrochloride are the preferred acids since these compositions have generally favorable solubility characteristics. Since the amine reagents are normally used in low percentage solutions or emulsions (on the order of one-half to five percent), it is preferable to maintain the volume of water sufficiently high to initially produce the low percent solutions without adding more water. It has been found satisfactory, however, to prepare concentrated solutions and then add water to such a concentrated solution prior to the use of the solution as a flotation reagent. The concentrated amine produced by either com.- position methods are easily stored and are not subject to deterioration.
While the invention has been illustrated by reference to specific illustrations, there is no intent to limit the spirit or scope of the invention to the precise details so set forth except insofar as defined in the following claims.
I claim:
1. In a process for preparing a liquefied amine collector reagent for flotation separations, the steps of melting a minor quantity of a normally solid, high molecular weight aliphatic amine composition in a major quantity of water, and then introducing into the resultant liquor a sufiicient amount of an acid to react with not more than a stoichiometric amount of the amine present in the liquor, and forming therewith a water soluble salt of the amine whereby to form a stabilized aqueous amine composition containing at least about 1% by weight of the amine composition.
2. In a process for preparing a liquefied amine collector reagent for flotation separations, the steps of melting a minor quantity of a normally solid, high molecular weight aliphatic amine composition in a major quantity of water, and then introducing into the resultant liquor a sufiicient amount of an acid to react with not more than a stoichiometric amount of the amine present in the liquor, and forming therewith a water soluble salt of the amine whereby to form a stabilized aqueous amine composition containing from about 1-5% by weight of the amine composition.
3. A process according to claim 2 in which about one-third equivalent of a stoichiometric amount of acid is used so as to form a stabilized composition.
4. A process according to claim 3 in which the acid is acetic acid.
5. A process according to claim 3 in which the acid is hydrochloric acid.
6. A process according to claim 3 in which the acid is nitric acid.
'7. A process according to claim 3 in which the acid is formic acid.
8. A process according to claim 3 in which the acid is hydrobromic acid.
9. In a process for preparing a liquefied amine collector reagent for flotation separations, the steps of melting a minor quantity of a normally solid, high molecular weight aliphatic amine composition in a major quantity of water, and then introducing into the resultant liquor a stoichiometric amount of an acid which'reacts with the amine present in the liquor to form a soluble salt thereof, whereby to form an aqueous stabilized amine salt solution.
10. A process according to claim 9 in which the acid is acetic acid.
11. A process according to claim 9 in which the acid is hydrochloric acid.
12. A process according to claim 9 in which the acid is formic acid.
13. A process according to claim 9 in which the acid is nitric acid.
14. A process according to claim 9 in which the acid is hydrobromic acid.
15. In a process for preparing a liquefied amine collector reagent for flotation separations, the steps of melting a minor quantity of a normally solid, high molecular weight aliphatic amine composition in a major quantity of water, and then introducing into the resultant liquor about 30% of a stoichiometric amount of acetic acid which reacts with the amine present in the liquor to form a soluble amine acetate salt, and thereby form an aqueous, stabilized amine composition containing at least about 1% of the amine composition by weight.
16. In a process for preparing a liquefied amine collector reagent for flotation separations, the steps of melting a minor quantity of a normally solid, high molecular weight aliphatic amine composition in a major quantity of water, and then introducing into the resultant liquor about 30% of a stoichiometric amount of hydrochloric acid which reacts with the amine present in the liquor to form a soluble amine chloride salt thereof, and thereby form m aqueous stabilized amine composition containing at. least about 1% of the amine composition by weight.
17. In a process of preparing a liquefied amine collector reagent for flotation separations, the steps of melting a minor quantity of an aliphatic amine composition in a major quantity of water, and then introducing into the resultant liquor a sufficient quantity of acetic acid to react with substantially all of the amine where-'- by to form a stabilized amine acetate in water solution.
18. A process according to claim 17 in which the amount of amine is not more than about. 5% by weight of the amount of water.
19. In a process of preparing a liquefied amine collector reagent for flotation separations, the steps of melting a minor quantity of an aliphatic amine composition in a major quantity of water, and then introducing into the resultant liquor substantially less than a stoichiometric amount of acetic acid to react with a portion of the liquefied amine whereby to form a stabilized emulsion of the aliphatic amine in an aliphatic amine acetate-' water solution.
20. In a process of preparing a liquefied amine collector reagent for flotation separations, the steps of melting not more than about 5% by weight of an aliphatic amine composition in at least about by weight of water, and then introducing into the resultant liquor substantially less than a stoichiometric amount of acetic acid to react with a portion of the liquefied amine whereby to form a stabilized emulsion of the aliphatic amine in an aliphatic amine acetate-water solution.
References Cited in the file of this patent UNITED STATES PATENTS The Chemistry of Fatty Amines, pamphlet pub. 194-3 by Armour Chemical Division, Armour and Company, Chicago, 111., 18 pages of text, 1 page reference.
Claims (1)
1. IN A PROCESS FOR PREPARING A LIQUEFIED AMINE COLLECTOR REAGENT FOR FLOTATION SEPERATIONS, THE STEPS OF MELTING A MINOR QUANTITY OF A NORMALLY SOLID, HIGH MOLECULAR WEIGHT ALIPHATIC AMINE COMPOSITION IN A MAJOR QUANTITY OF WATER, AND THEEN INTRODUCING INTO THE RESULTANT LIQUOR A SUFICIENT AMOUNT OF AN ACID TO REACT WITH NOT MORE THAN A STOICHIOMETRIC AMOUNT OF THE AMINE PRESENT IN THE LIQUOR, AND FORMING THEREWITH A WATER SOLUBLE SALT OF THE AMINE WHEREBY TO FORM A STABILIZED AQUEOUS AMINE COMPOSITION CONTAINING AT LEAST ABOUT 1% BY WEIGHT OF THE AMINE COMPOSITION.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US136740A US3034985A (en) | 1961-09-08 | 1961-09-08 | Amine flotation reagent preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US136740A US3034985A (en) | 1961-09-08 | 1961-09-08 | Amine flotation reagent preparation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3034985A true US3034985A (en) | 1962-05-15 |
Family
ID=22474157
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US136740A Expired - Lifetime US3034985A (en) | 1961-09-08 | 1961-09-08 | Amine flotation reagent preparation |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US3034985A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3520820A (en) * | 1964-10-30 | 1970-07-21 | Grace W R & Co | Cold water dispersible emulsions of filming amines |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1096459A (en) * | 1953-12-14 | 1955-06-21 | Prod Chim Ind Et Organiques So | Products based on fatty amines and their application to mineral flotation |
| US2816870A (en) * | 1954-07-19 | 1957-12-17 | Gen Mills Inc | Dispersible fatty amines |
-
1961
- 1961-09-08 US US136740A patent/US3034985A/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1096459A (en) * | 1953-12-14 | 1955-06-21 | Prod Chim Ind Et Organiques So | Products based on fatty amines and their application to mineral flotation |
| US2816870A (en) * | 1954-07-19 | 1957-12-17 | Gen Mills Inc | Dispersible fatty amines |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3520820A (en) * | 1964-10-30 | 1970-07-21 | Grace W R & Co | Cold water dispersible emulsions of filming amines |
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