CN114703013A - Method for removing residual cobalt ions in Cu-Zn-Co coating steel cord wet drawing wetting liquid - Google Patents

Abstract

The invention relates to the technical field of steel cord production, and discloses a method for removing residual cobalt ions in a Cu-Zn-Co coating steel cord wet drawing liquid. Obtain cobalt-removing pre-liquid, add cobalt-removing agent to the cobalt-removing pre-liquid; 2) the cobalt-removing agent reacts with the lubricating liquid, and separates the solid-liquid to obtain the cobalt-removing liquid and the cobalt-containing precipitate; 3) adding the cobalt-removing liquid to the cobalt-removing liquid Sodium hydroxide solution, adjust the pH value of the solution after cobalt removal to 10.5-11.6. In the method for removing residual cobalt ions in the wet drawing solution of Cu-Zn-Co coated steel cords, a cobalt-removing agent is added to the lubricating solution, and a preliminary cobalt removal is performed, and then it is reacted with a sodium hypochlorite solution under sunlight, Then, the precipitate obtained by the reaction is removed by filtration, so as to remove cobalt in the cobalt-containing lubricating fluid. The removal effect of cobalt ions is good. demand.

Description

A method for removing residual cobalt ions in a Cu-Zn-Co coating steel cord wet drawing solution

technical field

The invention relates to the technical field of steel cord production, in particular to a method for removing residual cobalt ions in a Cu-Zn-Co coating steel cord wet drawing solution.

Background technique

When the steel cord is drawn from coarse to fine diameter, it needs to be lubricated by lubricating liquid, because the steel cord already has a coating (copper-zinc-cobalt) before lubrication. After the steel cord is lubricated, the liquid of the lubricating liquid will Residual copper ion, zinc ion and cobalt ion, among them, lubricating oil is mainly composed of lubricating oil (fatty acid) + active agent + extreme pressure agent, etc., wherein lubricating oil (fatty acid) is the main body of lubrication, and the others are auxiliary components.

The production process of steel cord is mainly divided into four steps: dry drawing-heat treatment electroplating-wet drawing-twisting rope; It is called dry drawing, dry drawing is relatively less demanding) to 1.5mm-2.0mm; heat treatment and electroplating: the steel wire after dry drawing is heat treated, and then plated with Cu, Co, Zn to form a Cu-Zn-Co coating; wet drawing: The steel wire with Cu-Zn-Co coating should be finely drawn to a fine wire of 0.175-0.38mm. This step requires high drawing. The only drawing lubricating medium used is lubricating fluid, and the steel wire is carried out in the lubricating fluid. Drawing; twisting rope: twisting the steel wire into the form of a steel wire rope; in the above wet drawing process, Cu, Zn, and Co will enter the lubricating fluid during the drawing process, and too much of these ions will affect the lubricating fluid. The drawing effect of the subsequent steel wire, so these ions need to be removed to improve the drawing effect, and for Cu and Zn ions, there are mature removal methods, for the removal of Co, the existing technology is not yet mature, therefore, propose a A method for removing residual cobalt ions in a wet drawing solution for Cu-Zn-Co coated steel cords.

SUMMARY OF THE INVENTION

(1) Technical problems solved

In view of the deficiencies of the prior art, the present invention provides a method for removing residual cobalt ions in the wet drawing solution of Cu-Zn-Co coated steel cords, which has the advantages of high removal efficiency of cobalt ions and solves the problem of traditional wet drawing of steel cords. The problem of low removal efficiency of residual cobalt ions in the lubricating solution.

(2) Technical solutions

In order to achieve the purpose that the above-mentioned cobalt ion removal efficiency is high, the present invention provides the following technical solutions: a method for removing residual cobalt ions in a Cu-Zn-Co coating steel cord wet drawing solution, comprising the following steps:

1) First remove copper and zinc from the lubricating fluid, and remove the partition to obtain a pre-cobalt-removing solution, and add a cobalt-removing agent to the pre-cobalt-removing solution;

2) The cobalt-removing agent reacts with the lubricating liquid, and separates the solid-liquid to obtain the cobalt-removing liquid and the cobalt-containing precipitate;

3) adding sodium hydroxide solution to the solution after removing cobalt, adjusting the pH value of the solution after removing cobalt to 10.5-11.6;

4) then add sodium hypochlorite solution, and react under sunlight to obtain precipitate;

5) Filtration of the above solution to remove precipitates to obtain a lubricating liquid from which cobalt ions are finally removed.

Preferably, the concentration of cobalt in the cobalt-containing lubricating fluid is 5 mg/L to 100 mg/L, and the reaction time between the sodium hypochlorite solution and the solution after removing cobalt is 5-8 hours.

Preferably, the cobalt removing agent is composed of dimethyl dithiocarbamate and sodium nitrite, and the mass ratio of its dimethyl dithiocarbamate to sodium nitrite is 12-18:1- 5.

Preferably, the reaction temperature of the cobalt removing agent and the lubricating liquid is 80-95° C., the reaction time is 1-2 h, and the reaction is carried out in a mixer with a stirring speed of 500-700 rpm.

Preferably, the mass concentration of the sodium hydroxide solution is 25%-35%, and the mass concentration of the sodium hypochlorite solution is 10-20%.

Preferably, the lubricating liquid is electrolytically precipitated to remove copper and zinc.

(3) Beneficial effects

Compared with the prior art, the present invention provides a method for removing residual cobalt ions in a Cu-Zn-Co coating steel cord wet drawing solution, which has the following beneficial effects:

The method for removing residual cobalt ions in the wet drawing solution of Cu-Zn-Co coated steel cords is to add a cobalt removing agent to the lubricating solution, and perform preliminary cobalt removal, and then react it with sodium hypochlorite solution under sunlight, Then, the precipitate obtained by the reaction is removed by filtration, thereby removing cobalt in the cobalt-containing lubricating fluid. The removal effect of cobalt ions is good. demand.

Detailed ways

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

Embodiment 1: A method for removing residual cobalt ions in a Cu-Zn-Co coating steel cord wet drawing solution, comprising the following steps:

1) First, remove copper and zinc from the lubricating fluid, and remove the partition to obtain a pre-cobalt-removing solution. The lubricating fluid removes copper and zinc by electrolytic precipitation, and adds a cobalt-removing agent to the pre-cobalt-removing solution. The composition of thiocarbamate and sodium nitrite, the mass ratio of dimethyl dithiocarbamate to sodium nitrite is 12:1, and the concentration of cobalt in the cobalt-containing lubricating fluid is 5mg/L;

2) The cobalt-removing agent reacts with the lubricating liquid, and the solid-liquid separation is performed to obtain the cobalt-removing liquid and the cobalt-containing precipitate. The reaction temperature of the cobalt-removing agent and the lubricating liquid is 80 °C, and the reaction time is 1 h, and the reaction is carried out in a mixer. The stirring speed is 500 rpm;

3) adding sodium hydroxide solution to the solution after removing cobalt, the mass concentration of sodium hypochlorite solution is 10%, adjusting the pH value of the solution after removing cobalt to 10.5, and the mass concentration of sodium hydroxide solution is 25%;

4) Then add sodium hypochlorite solution, the reaction time of sodium hypochlorite solution and the solution after removing cobalt is 5h, and react under sunlight to obtain precipitate;

5) Filtration of the above solution to remove precipitates to obtain a lubricating liquid from which cobalt ions are finally removed.

Embodiment 2: a method for removing residual cobalt ions in a Cu-Zn-Co coating steel cord wet drawing solution, comprising the following steps:

1) First, remove copper and zinc from the lubricating fluid, and remove the partition to obtain a pre-cobalt-removing solution. The lubricating fluid removes copper and zinc by electrolytic precipitation, and adds a cobalt-removing agent to the pre-cobalt-removing solution. The composition of thiocarbamate and sodium nitrite, the mass ratio of dimethyldithiocarbamate to sodium nitrite is 15:3, and the concentration of cobalt in the cobalt-containing lubricating fluid is 50 mg/L;

2) The cobalt-removing agent reacts with the lubricating liquid, and the solid-liquid separation is performed to obtain the cobalt-removing liquid and the cobalt-containing precipitate. The reaction temperature of the cobalt-removing agent and the lubricating liquid is 90 ° C, and the reaction time is 1.5 h, and the reaction is carried out in a mixer with stirring. The speed is 600 rev/min;

3) adding sodium hydroxide solution to the solution after removing cobalt, the mass concentration of sodium hypochlorite solution is 15%, adjusting the pH value of the solution after removing cobalt to 10.55, and the mass concentration of sodium hydroxide solution is 30%;

4) Then add sodium hypochlorite solution, the reaction time of sodium hypochlorite solution and the solution after removing cobalt is 6h, and react under sunlight to obtain precipitate;

5) Filtration of the above solution to remove precipitates to obtain a lubricating liquid from which cobalt ions are finally removed.

Embodiment 3: a method for removing residual cobalt ions in a Cu-Zn-Co coating steel cord wet drawing solution, comprising the following steps:

1) First, remove copper and zinc from the lubricating fluid, and remove the partition to obtain a pre-cobalt-removing solution. The lubricating fluid removes copper and zinc by electrolytic precipitation, and adds a cobalt-removing agent to the pre-cobalt-removing solution. The composition of thiocarbamate and sodium nitrite, the mass ratio of dimethyl dithiocarbamate to sodium nitrite is 118:5, and the concentration of cobalt in the cobalt-containing lubricating fluid is 100 mg/L;

2) The cobalt-removing agent reacts with the lubricating liquid, and the solid-liquid separation is performed to obtain the cobalt-removing liquid and the cobalt-containing precipitate. The reaction temperature of the cobalt-removing agent and the lubricating liquid is 95 ° C, and the reaction time is 2 h, and the reaction is carried out in a mixer. The stirring speed is 700 rpm;

3) adding sodium hydroxide solution to the solution after removing cobalt, the mass concentration of sodium hypochlorite solution is 20%, adjusting the pH value of the solution after removing cobalt to 11.6, and the mass concentration of sodium hydroxide solution is 35%;

4) Then add sodium hypochlorite solution, the reaction time of sodium hypochlorite solution and the solution after removing cobalt is 8h, and react under sunlight to obtain precipitate;

5) Filtration of the above solution to remove precipitates to obtain a lubricating liquid with cobalt ions removed in the end.

Experimental example:

Take 2000mL of cobalt-containing lubricating fluid with a cobalt concentration of 29.5mg/L, add a cobalt-removing agent to make a preliminary reaction, remove the reacted precipitate, adjust the pH value, and then add the initial cobalt-removing solution to a concentration of 30% Then, the cobalt-removing lubricating fluid is measured, and the cobalt-removing rate is over 95%, which meets the needs of wet drawing of steel cords.

Judgment standard: the cobalt-containing lubricating fluid treated by the present invention can be detected by atomic absorption spectrometry (AAS) or by inductively coupled plasma dispersion spectrometer ICP-OES.

The beneficial effects of the invention are as follows: adding a cobalt removing agent to the lubricating liquid, and performing preliminary cobalt removal, then reacting it with a sodium hypochlorite solution under sunlight, and then filtering and removing the precipitate obtained by the reaction, thereby removing the cobalt-containing lubricating liquid The cobalt and cobalt ions have a better removal effect, which can meet the needs of wet drawing of steel cords.

Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, and substitutions can be made in these embodiments without departing from the principle and spirit of the invention and modifications, the scope of the invention is defined by the appended claims and their equivalents.

Claims (6)

1. A method for removing residual cobalt ions in a Cu-Zn-Co coating steel cord wet drawing wetting liquid is characterized by comprising the following steps:

1) firstly, removing copper and zinc from the lubricating liquid, and performing separation treatment to obtain a cobalt-removing precursor liquid, and adding a cobalt-removing agent into the cobalt-removing precursor liquid;

2) the cobalt removing agent reacts with the lubricating liquid, and solid-liquid separation is carried out to obtain cobalt-removed liquid and cobalt-containing precipitate;

3) adding a sodium hydroxide solution into the cobalt-removed solution, and adjusting the pH value of the cobalt-removed solution to 10.5-11.6;

4) then adding a sodium hypochlorite solution, and reacting in the sun to obtain a precipitate;

5) and filtering the solution to remove precipitates to obtain the lubricating liquid finally removing the cobalt ions.

2. The method for removing the residual cobalt ions in the wet drawing liquid for the Cu-Zn-Co coated steel cord as claimed in claim 1, wherein the concentration of cobalt in the cobalt-containing lubricating liquid is 5mg/L to 100mg/L, and the reaction time of the sodium hypochlorite solution and the solution after cobalt removal is 5 to 8 hours.

3. The method for removing the residual cobalt ions in the wet drawing liquid for the Cu-Zn-Co coated steel cord as claimed in claim 1, wherein the cobalt removing agent is composed of dimethyldithiocarbamate and sodium nitrite, and the mass ratio of dimethyldithiocarbamate to sodium nitrite is 12-18: 1-5.

4. The method for removing the residual cobalt ions in the wet drawing liquid for the Cu-Zn-Co coated steel cord as claimed in claim 1, wherein the reaction temperature of the cobalt removing agent and the lubricating liquid is 80-95 ℃, the reaction time is 1-2h, and the reaction is carried out in a stirrer with a stirring speed of 500-700 rpm.

5. The method for removing the residual cobalt ions in the wet drawing solution for the Cu-Zn-Co coated steel cord as claimed in claim 1, wherein the mass concentration of the sodium hydroxide solution is 25% -35%, and the mass concentration of the sodium hypochlorite solution is 10% -20%.

6. The method for removing the residual cobalt ions in the wet drawing liquid for the Cu-Zn-Co coated steel cord as claimed in claim 1, wherein the lubricating liquid is used for removing copper and zinc which are separated out by electrolysis.