US2303962A - Concentration of mica - Google Patents

Description

Patented Dec. 1, 1942 CONCENTRATION OF MICA Francis X. Tartar-on and Allen T. Cole, Mulberry,

Fla, assignors to Phosphate Recovery Corporation, New York, N. Y., a corporation of Delaware No Drawing.

9 Claims.

This invention relates to a froth-flotation process for the concentration of mica from mixtures containing mica and impurities such as clay, feldspar, quartz and silicious material. The general object of the invention is to produce a clean, bright,' mica concentrate containing negligible clay or grit and having a weight per cubic foot acceptable to the trade. Such weight of mica concentrates is usually required by the trade to be less than 20 lbs. per cubic foot; and this is attained by the use of the invention hereinafter described.

The usual fatty acids and their soaps when used alone have been found to be ineffective for the concentration of mica by froth-flotation of the mica. Tartaron and Harrison, assignors to the same assignee to which the present application is assigned, it is pointed out that an alkali resinate such as sodium resinate is an effective agent for the concentration of mica by froth-flotation.

The processes for concentrating mica hereinafter described are the result of several discoveries. One -of these discoveries is that by the use of certain inorganic compounds which act as activating agents, not only are improved results obtained when an alkali resinate such as sodium resinate is employed as the flotation agent as described in said Tartaron and Harrison patent, but also that other anionic collectors are made effective for the froth-flotation of mica. These activating agents are salts and bases of the alkaline earth metals, including calcium, barium, magnesium and strontium, and their compounds including hydroxides, carbonates, chlorides, etc. Capable of employment in conjunction with these activators are anionic collectors such as fatty acids, resin acids, naphthenic acids, tall oils and their soaps. Frothers such as pine oil or pine tar oils such as P. T. 101 may also be of assistance in concentrating mica by froth-flotation with the use of'the activating agents and flotation agents which have been mentioned.

We have also discovered that pre-agitation of the mica ore pulp with water prior to addition of reagents efiects improved results. Our belief is that this may be due to the breaking up of books Application May 21, 1941, Serial No. 394,498

' treated in the same manner if desired.

In U. S. Patent No. 2,226,103 to The following examples illustrate the process of the present invention. The material treated was a micaceous product derived from the washer of Kaolin, Inc., at Spruce Pine, N. C. The mica present was muscovite intermixed with clay, feldspar, quartz and silicious material. The examples merely illustrate the processes of the in vention and are not to be construed as limiting its scope. All cubic weight figures are in pounds per cubic foot.

Examples 1 and 2 are comparative and show the beneficial effect of employing lime as an activator in connection with an alkali resinate such as sodium resinate.

Example 1.No activator.A charge of micaceous material, known as sand box paper clay derived from Kaolin, Inc., was placed in a frothiiotation machine and diluted to form a pulp of about 10% solids. To this pulp was added sodium resinate in the amount of 5 lbs. per ton of solids in the pulp, and pine oil in the-amount of 0.42' lb. per ton of such solids. After brief agitation in the froth-flotation machine a rougher froth was produced; and this rougher froth was diluted with water and a cleaner froth-float was made therefrom without any further addition of agents. Tailings of this second operation were considered middlings which would be returned to the rougher flotation machine. The results were as follows:

of prod.

Example 2.With lime as an activator.The operations of Example 1 were repeated, except that 1.5 lbs. of lime per ton of solids in the feed were added to the pulp which was then subjected to brief agitation, after which the sodium resinate .and pine oil were added in the same quantities as in Example 1, and the thus conditioned pulp was subjected to the same treatments as in the case of Example 1. The were as follows:

It will be noted that while the recovery in Example 2 is somewhat less than in Example 1 thegrade of mica concentrate was improved from 19.00 lbs. to 14.13 lbs. per cubic foot. Thus it is obvious that the use with sodium resinate of lime as an activator gives highly beneficial results.

The following Examples "3 and 4 illustrate the beneficial effect of pre-agitation of the ore pulp with water. before addition of the activating and flotation agents. These tests were made on another sample of fsand box settlings also obtained from Kaolin, Inc.

Example 3.No pre-agitation with water.-A charge of "sand box settlings also obtained from Kaolin, Inc. was placed in a froth-floation machine as a pulp at about 40% solids. To this charge was added 2.5 lbs. of lime per ton of solids in the feed, after which the pulp was subjected to brief agitation; and then there were added 6.0 lbs. of sodium resinate and 0.42 lb. of pine 011, both per ton of solids in the feed. and the pulp was again subjected to brief agitation. After diluting this conditioned pulp to about 10% solids, a rougher froth-float was produced. This rougher frothfloat was returned to the flotation machine, and to it were added 0.4 lb. of lime and 0.14 lb. of pine oil, both per ton of solids in the original feed; and after dilution a cleaner froth-float was made. This cleaner froth-float was also returned to the machine, and to it were added 0.3 lb. of lime and 0.14 lb. of pine oil. both per ton of solids in the original feed; and after suitable dilution a recleaner froth-float. was produced. The results were as follows:

Percent Products wt.of

feed

Feed 100.0 ma (lone 28.9 11.4 Mlds-2 111 22.9 Mids-I 10.4 25.1 Tails I 54.0 31.0

Example 4.Pre-agitation with water.--The treatments in this example were identical with Example 3, except that the ore pulp at about 40% solids was agitated for aboutlo minutes in the froth-flotation machine prior to the initial or first addition of the lime. The results were as follows:

Per cent cm wt Products g of prod.

rm! 100.0 20. 3 Com 30. 6 16.8 Mids-2 M 25.1 Mids-l 1o. 9 2a 1 ails. as. 1 32.1

It will be apparent that the recovery in Example 4 was slightly better than in Example 3; and that the grade of mica concentrate was improved from 17.4 lbs. to 15.8 lbs. per cubic foot; thereby proving that pre-agitation of the mica or pulp before adding the agents was beneficial.

The following Examples 5, 6 and 7 illustrate the'successful use of various fatty acids in conjunction with lime, in froth-flotation concentration of mica.- In these examples, the amount of lime was 2.5 lbs. and the amount of. pine oil was 0.28 lbs. both per ton of solids in the feed. In

. each example the material treated was sand box .settlings obtained from Kaolin, Inc.

Example 5.--A pulp containing the material to be treated in the amount of about 500 g. at 40% solids was agitated in a laboratory flotation machine for about 10 minutes. Then the lime was added and the pulp was again briefly agitated. To the pulp was then added 4.03 lbs. of Upjohn's fatty acid (an animal fatty acid) per ton of solids in the original feed together with the pine oil;

after which the pulp was again briefly agitated.

After diluting the thus conditioned pulp to about 10% solids, a rougher froth-float was produced and removed. This rougher froth was returned to the machine, 0.40 lb. of lime per ton of solids in the originalfeed was added, and after suitable dilution a cleaner froth-float was made. This cleaner froth was also returned to the machine, treated with 0.30 lb. of lime per ton of solids in the original feed, diluted and a final mica frothfloat was made. The results were as follows:

Per cent Cu. wt

Products wtegi prod Feed 100. 0 26. 8 Cone 24. 9 l5. 5 Mids-2 5. 7 24. 5 Mids-l 12.8 as 2 Tails 66. 0 29.0

Conc.+Midse2 30. 6 17. 2

Example 6. 'Ihe treatments in this example were identical with Example 5, except that 4.99 lbs. of red oil (crude oleic acid) was used instead of Upjohn's fatty acid. The results were as follows:

Per cent Cubic Product wt. of wt. of

feed prod.

Feed 100. 0 20. 3 Cone l8. 5 l5. 1 Mills-2 5. 3 22. 4 Mids-l 12. 8 20. 0 Tails I 03. 4 a0. 0 Cono.+Mid-2 at 1111 Example 7..The treatments in this example were identical with Examples 5 and 6, except that, as the fatty acid, 3.07 lbs. of Chatham fatty acid was used. This fatty acid is a tall 011- or paper mill by-product containing resin acids and vegetable fatty acids. The results were as fol- It will be noted that in each of Examples 5, 6 and 7 a mica concentrate was produced the weight of which was considerably below 20 lbs. per cubic foot; thereby provingthat various fatty acids,

when used in conjunction with lime as an activator, result in satisfactory concentration of mice. by froth-flotation.

The following Examples 8, 9, 10 and 11 illustrate the successful use with a fatty acid of the activating agents, of the kind hereinbefore mentioned, such as calcium chloride, magnesium carbonate, barium hydroidde and strontium hydroxide. In each of these examples, Chatham fatty acid to the amount of 3.07 lbs. and pine oil in the amount of 0.28 lb., both per ton of solids in the feed, were employed. The material treated was again sand box settlings obtained from Kaolin, Inc.

Example 8.A charge of about 500 g. of the material to be treated was agitated in a flotation machine for about 10 minutes at 40% solids. Then 8.75 lbs. of calcium chloride per ton of solids in the pulp was added, after which the pulp was again briefly agitated. Then the Chatham fatty acid and pine oil were added and the pulp was conditioned. The pulp was then diluted to about 10% sollds'and a mica frothfloat was made and removed. The results were as follows:

Example 9.-In this treatment, the activator was magnesium carbonate in the amount of 2.85 lbs. per ton of solids in the pulp which was briefly agitated prior to the addition of the fatty acid and pine oil with which the pulp was then conditioned. The thus conditioned pulp was sub- Jected to froth-flotation and a rougher mica froth-float was removed. This rougher froth was subjected to a cleaner froth-flotation treatment after the addition to it of 0.46 lb. of magnesium carbonate per ton of solids in the original feed; and the froth-float thus obtained was subjected to re-cleaner froth-flotation treatment after the addition of 0.34 lb. of magnesium carbonate per ton of solids in the orignal feed. The results of these operations were as follows:

Per cent Cubic wt. Pmdu'ct wt. oifeed of prod.

100. 26. 3 2i. 9 l5. 8 8. 7 23.9 19. l 29. 3 50. 3 30. l

Conc.+Mids-2 30. 6 18. 1

Example 10.The treatments in this example were the same as in Example 9, except that the activator used was barium hydroxide to the amount of 5.78 lbs. in the rougher treatment, 0.93 lb. in the cleaner treatment and 0.67 lb. in the re-cleaner treatment, all per ton of solids in the original feed. The results were as follows:

Example 11.-The treatments in this example were the same as in Example 9, except that the activator was strontium hydroxide which was added to the amounts of 6.64 lbs. in the rougher treatment, 4.26 lbs. in the cleaner treatment, and 3.19 lbs. in the re-cleaner treatment, all per ton of solids in the original feed. The results were as follows:

Per cent Cubic wt. I wt. oileed oi prod.

Feed 100. 0 26. 3 Cone 27. 8 l6. 9 5. 4 22. 9 ll. 4 30. 6 55. 4 30. 5

Conc.+Mids-2 33. 2 l7. 9

Example 12.'-In this treatment, as in Example 9, the activator was magnesium carbonate, but

the flotation agent was sodium resinate which Per cent Cubic Product wt. of wt. oi

teed prod.

Feed .L 100.0 25.3 Conc.. 22. 7 l6. 4 MldS-Z--- 4.6 22.1 Mids-l--- 7.7 27.4 I ails cs0 30.8

Conc.+Mids-2 27. 3 l7. 3

The following Examples 13 and 14 show successful concentration of mica by froth-flotation of the mica by the use, with lime as an activating agent, of sodium oleate or naphthenic acid. As before, the mica material treated was sand box settlings obtained from Kaolin, Inc.

Example 13.-An aqueous pulp of the mica ore was agitated in a froth-flotation machine for about ten minutes at 40% solids, diluted to 10% solids; and then again briefly agitated with lime to the amount of 3.80 lbs. per ton of solids in the feed. To this pulp were added 6.00 lbs.

of sodium oleate and 0.42 lb. of pine oil, both per ton of solids in the feed, and the pulp was then subjected to brief agitation. The thus conditioned pulp was subjected to froth-flotation and a rougher mica froth-float was removed. This rougherfroth after being reconditioned with 0.70 lb. of lime and 0.28 lb. of

- pine oil, both per ton of solids in the original feed. was subjected to froth-flotation to produce the final mica concentrate in the froth-float. The results were as follows:

Per cent Cubic Product wt. of wt. of

feed prod Conc.+Mids 36. 6 19. 3

Example 14.-An adueous pulp of the mica ore was agitated in a. froth-flotation machine for about ten minutes at 40% solids; and then lime, to the amount of 2.50 lbs. per ton of solids in the feed, was added and the pulp was again briefly agitated. To this thick pulp were added naphthenic acid to the amount of 6.00 lbs., pine oil to the amount of 0.42 11)., both per ton of solids in the feed, and the pulp was then agitated for about two minutes. After dilution to solids, the thus conditioned pulp was subjected to froth-flotation and a rougherfrothfloat was removed. This rougher froth, after reconditioning with 0.40 lb. of lime and 0.28 lb. of pine oil, both per ton'of solids in the ori inal feed, was subjected to froth-flotation and a first cleaner froth-float was removed; and this cleaner froth-float, .atter reconditioning with 0.30 lb. of lime and 0.28 lb. of pine 011, both per ton of solids in the original feed, was subjected' to froth-flotation to produce 'the final concentrate. The results were as follows:

From the foregoing Examples 8 to 14 inclusive, it will be apparent that the activators hereinbefore mentioned, of which lime, calcium chloride, magnesium carbonate, barium hydroxide and strontium hydroxide are examples, permit the' use of fatty acids, naphthenic acids, resin acids and their soaps in the froth-flotation concentration of mica.

-silicious material,

What is claimed is:

1. The process for the concentration of mica from a mixture of mica with impurities 'comprising principally clay, feldspar, quartz and comprising adding to an aqueous pulp of such .micaceous mixture a reagent consisting of an' inorganic compound of an alkaline earth .metal serving as an activator for .the mica together with an anionic collector, and separating the mica from said mixture by froth-flotation of the mica away from the other ingredients of-the mixture.

2. The-process of claiml, in which the aqueous pulp is agitated prior to the addition of reagents.

Q 3. The pl Qcss of claim 1, in which the inorganic compound is selected from the class consisting of oxides and hydroxides of alkaline earth metals. 4

4. The process of cla 1', in which the inorganic compound is lime.-

5. The process of claim 1. in whi'chthe inorganic compound is magnesiumcarbonate.

6. The process ofclaim '1, in which'the'inorganic compound is barium hydroxide.

7. The process of claim 1; in which'the'a'nionic collector-is selected from the group consisting of fatty acids, resin acids, oils and their soaps.

- 8. The process of claim 1, in which a frother is employed in conjunction with the activator andcollecton-v- 9. The process of claim 1, in which the reagents are added in tion treatments.

naphthenic acids, tall more x TARTARON. mm '1'. com.

steps to a plurality of dots-- CERTIFICATE; OF combmmn; Patent 110. 2,505,962. December 1', 19!;2.

mncxs x. mnmnom', ET AL.

.It is hereby oertitied'that error appeara-i'in'the prgited specification of the above numbered patent requiriqg correction as tfolloyva: Page 1,flr'et column, line 21, after Broth-flotation and before the period insert--01 the mica-:; page 1 .tfiretf' oolunih, line 10, "after *rougher' insert -"-m1ca lines 18- and 1-9, for "final concentrate read final mica concentrate in thefroth-floht-q and that the said. Letters Patent shoplq be readwith t i correctiqn thereip that the same IhB-Y conform to the record or the case 1n ,the Patent Office.

Signed a sealer} this 19th day of January, A, n. 191;

(Seell' --He nry Van Arsdale, v

- .Aeting Commissioner of Patents.