RU2236907C1 - Foaming agent for floatation of ores of non-ferrous metals and method of production of foaming agent - Google Patents

Abstract

FIELD: concentration of minerals; floatation of ores of non-ferrous metals.

SUBSTANCE: proposed foaming agent contains dimethyl (isopropynyl ethynyl) carbinol and diisopropynyl acetylene at the following relationship of components, mass-%: dimethyl (isopropynyl athynyl) carbinol, 85-94; diisopropynyl acetylene, 6- 15. Tetramethyl butadion is treated by aqueous solution of acid boiling point of reaction mixture in presence of inhibitor of radical polymerization; vapor thus formed is mixture of water steam and organic component which is distilled and condensed; organic layer is separated and rectification is performed at atmospheric pressure collecting fraction at boiling point of 115-180 C. It is good practice to use 15-% solution of phosphoric acid for treatment of tetramethyl butadion; hydroquinone in the amount of 0.15 mass-% shall be used as inhibitor of radical polymerization.

EFFECT: increased degree of extraction of useful component; reduced consumption of foaming agent.

4 cl, 4 tbl, 3 ex

Description

The invention relates to the field of mineral processing and can be used for flotation of non-ferrous metal ores.

Currently, flotation of non-ferrous metal ores, as a rule, use compositions consisting of a collector and a foaming agent. As a collector, heteropolar sulfur-containing organic compounds, for example, butyl aeroflot, various xanthates, dimethyl carbamate, etc., are usually used. Waste from various chemical industries is sometimes used as a foaming agent; pine oil is also used.

It is also known (Preliminary patent of the Republic of Kazakhstan No. 7383, bull. No. 4, 04/15/99) the use of dimethyl (isopropenylethynyl) carbinol (DMIPEC) as a foaming agent, which made it possible to slightly increase the degree of extraction of copper, lead, zinc in the flotation process.

In the work (RF patent No. 2198034, publ. 10.02.03, prototype) a foaming agent is proposed, which is a mixture (wt.%):

Dimethyl (isopropenylethynyl)

carbinol (DMIPEK) 95.0-98.0

Tetramethylbutinediol (TMBD) 0.1-1.5

Diisopropenylacetylene (DIPA) 0.1-1.0

2,5-dimethyl-1,4-hexadiene-3-one

(DMGDO) 1.5-2.5

The foaming agent prototype is obtained as follows (RF patent 2198034, publ. 10.02.03, prototype). TMBD is treated with an aqueous acid solution in the presence of a radical polymerization inhibitor at the boiling point of the reaction mixture. The resulting foaming agent is distilled off with steam, then it is extracted from the distillate with an organic solvent and isolated from the organic layer by distillation in vacuo. The product yield is 55-72%.

Using a foaming agent-prototype allows, according to the authors, to increase the degree of extraction of non-ferrous metals and stabilize it at different temperatures and pH values of the flotation medium.

However, during the flotation of polymetallic ores, when flotation takes place in two or more stages, the urgent task is to develop reagents that selectively affect the extraction of various non-ferrous metals, i.e. allowing selectively increasing the degree of extraction of one metal, without changing (or decreasing) while the degree of extraction of another.

So, for example, the technological scheme of flotation of copper-nickel ore includes the initial copper flotation, the tailings from which are sent to nickel-pyrrhotite flotation. On copper flotation, it is desirable to extract copper as much as possible in the concentrate, and nickel to a lesser extent. At the nickel-pyrrhotite flotation stage, it is desirable to extract both nickel and copper as much as possible.

The present invention is the creation of a foaming agent that has a selective effect on the degree of extraction of various non-ferrous metals during flotation.

To solve this problem, a foaming agent for flotation of non-ferrous metal ores is proposed, including DMIPEK and DIPA in the following ratio of components (wt.%):

DMIPEK 85-94

DIPA 6-15

A method of obtaining the proposed composition includes treating TMBD with an aqueous acid solution in the presence of a radical polymerization inhibitor at the boiling point of the reaction mixture. The resulting steam, which is a mixture of water vapor and an organic component, is distilled off, condensed, the organic layer is separated and distillation is carried out at atmospheric pressure, collecting a fraction with a boiling point of 115-180 ° C.

Any acid, acid salt, or medium providing a pH of the reaction medium below 4 can be used as an aqueous acid solution, but for the target preparation of the inventive mixture, it is preferable to use a 15% phosphoric acid solution as an aqueous acid solution, and as a radical polymerization inhibitor, hydroquinone in an amount of 0.15 wt.%.

The yield of the target product will be greater if the organic layer before rectification is sent to drainage, and distillation is carried out in the presence of a radical polymerization inhibitor.

It is essential to obtain a foaming agent of the claimed composition is a distillation at atmospheric pressure and in the specified temperature range. In violation of these conditions, the resulting foaming agent has a different composition and does not have a selective effect during flotation.

Examples of carrying out the invention.

Example 1

In a 140 liter stainless steel reactor with a 140 rpm propeller stirrer, 80 liters of water, 1 liter of 98% phosphoric acid, 0.14 grams of hydroquinone and 15 kg of tetramethylbutinediol are charged. Mixing and heating are included. The azeotrope is distilled off at a speed of 60-70 liters per hour. After the azeotrope is distilled off, molten tetramethylbutinediol begins to be fed into the reactor at a rate of 15 kg per hour, as well as recycled water.

The flow of the hot azeotrope, passing through the heat exchanger, is cooled to a temperature of 50 ° C and goes to the separation of the aqueous and organic layers.

The water layer at a speed of 80 kg per hour is sent back to the reactor.

The organic layer at a speed of 10 kg per hour, passing through a column of sodium sulfate, is sent to a 200-liter storage tank. From it periodically, once every 15 hours, 150 kg of the mixture are loaded into the cube of the distiller, 0.225 kg (0.15%) of hydroquinone are added and the following fractions are distilled off:

- light fraction (up to 115 ° C) - 4.5 kg;

- the target fraction of dimethylisopropenylethynylcarbinol and diisopropenylacetylene (115-180 ° C) - 117 kg.

VAT residue in the amount of 28.5 kg is sent to the capacity of the source tetramethylbutinediol.

The light fraction is sent for recycling.

Using gas-liquid chromatography, it was found that the target fraction has the following composition:

- dimethylisopropenylethynylcarbinol - 88 wt.%;

- diisopropenylacetylene - 12 wt.%.

This fraction is sent to a 200-liter tank with an anchor mixer, to which 0.18 kg of hydroquinone is added and stirred for 2 hours. After mixing, the mixture is sent to the spill site of the finished product and then to the warehouse.

The proposed method for producing the inventive mixture is economically advantageous, it allows to immediately obtain as a marketable product a mixture of the composition of interest to us with a sufficient degree of purity, which is much more economically advantageous than using a mixture of 2 individual compounds.

Example 2

Flotation on the initial feed of the copper cycle of the processing plant of the Norilsk Mining and Metallurgical Combine was carried out under the following conditions and component costs (basic experience):

butyl aeroflot - 16 g / ton;

pine oil - 5 g / ton;

flotation time is 22 minutes.

The results of the basic experience are presented in the table below:

When replacing pine oil with a foaming agent obtained according to the previous example (DMIPEK - 88 wt.%, DIPA - 12 wt.%), Taken in an amount of 3 g / ton, and under the same other conditions, the following results were obtained:

A comparison of the results shows that the use of the inventive foaming agent allows you to:

- increase by 1.30% the degree of extraction of copper in concentrate,

- reduce by 0.35% the degree of extraction of Nickel,

- increase by 1.41 units. Ni: Cu ratio

- reduce the consumption of foaming agent by 40%.

Example 3

The basic experience in the 2nd stage of flotation - flotation on a nickel-pyrrhotite cycle was carried out under the following conditions and component costs:

additive DP-4 - 20 g / ton;

dimethyldithiocarbamate (DMDK) - 50 g / ton;

xanthate (KX) - 70 + 50 + 30 + 20 + 10 g / ton;

pine oil - 5 + 5 + 5 + 5 + 5 g / ton.

The results of the basic experience are presented in the table below:

When replacing pine oil with the mixture obtained according to example 1, in the indicated quantities and the following composition of the used reagents:

DP-4 - 20 g / ton;

DMDK - 50 g / ton;

KH - 35 + 25 + 15 + 10 + 5 g / ton;

the foaming agent of example 1 is 35 + 25 + 15 + 10 + 5 g / ton.

The following results were obtained:

The results show that at the second flotation stage, the degree of extraction of copper in concentrate increased by 0.79%, and the degree of extraction of nickel by 1.05%, while the consumption of xanthate decreased by 50%.

Thus, the selectivity of the inventive blowing agent can reduce the loss of Nickel with tailings flotation by 0.07%.

The use of the mixture at other ratios of reagents (beyond the stated intervals) increases the degree of extraction of non-ferrous metals, but does not lead to selectivity of action.

The selectivity of the inventive blowing agent is also manifested in the flotation of other non-ferrous ores, for example, lead-zinc.

Claims (4)

1. Foaming agent for flotation of non-ferrous metal ores, including dimethyl (isopropenylethynyl) carbinol and diisopropenylacetylene, characterized in that the said elements are contained in the following ratio of components, wt.%: Dimethyl (isopropenylethynyl) carbinol 85-94 Diisopropenylacetylene 6-15 2. The method of producing a foaming agent according to claim 1, characterized in that tetramethylbutinediol is treated with an aqueous acid solution at the boiling point of the reaction mixture in the presence of a radical polymerization inhibitor, the resulting vapor, which is a mixture of water vapor and an organic component, is distilled off, condensed, the organic layer is separated and carry out rectification at atmospheric pressure, collecting the fraction, with a boiling point of 115-180 ° C. 3. The method according to claim 2, characterized in that for the treatment of tetramethylbutinediol using a 15% solution of phosphoric acid. 4. The method according to claim 2, characterized in that as an inhibitor of radical polymerization using hydroquinone in an amount of 0.15 wt.%.