CN109395872B - Preparation method of hydrophobic molybdenum tailing powder - Google Patents
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Abstract
The invention discloses a preparation method of hydrophobic molybdenum tailing powder, which comprises the following steps: firstly, ball-milling molybdenum tailing slag by a wet method to obtain powder; secondly, drying the powder, and adding hydrochloric acid for immersion cleaning to obtain a mixture; thirdly, filtering the mixture, washing the trapped substance and drying; grinding and dispersing, and adding NaOH solution for immersion washing to obtain a mixture; fifthly, filtering the mixture, washing the trapped substance and drying; sixthly, preparing a hydrophobic modifier; seventhly, grinding the trapped substance, adding the trapped substance into a hydrophobic modifier, and stirring in a water bath to obtain a suspension; eighthly, filtering the suspension, drying the retentate, grinding by a dry method, and sieving to obtain the hydrophobic molybdenum tailing powder. The method organically combines ball milling, impurity removal and modification processes, so that the obtained hydrophobic molybdenum tailing powder has high activation degree and good hydrophobic property.
Description
Technical Field
The invention belongs to the technical field of mine solid waste recycling, and particularly relates to a preparation method of hydrophobic molybdenum tailing powder.
Background
With the rapid development of high and new technologies, the demand for metal molybdenum is increasing, and the continuous increase of the exploitation and utilization scale of molybdenum ore leads to the accumulation of a large amount of molybdenum tailings to be idle, which not only causes the great waste of resources, but also has profound influence on the environment. The new technology is actively developed, the solid wastes are subjected to high value-added utilization again, and the method has important significance for promoting national economic development and environmental improvement.
The molybdenum tailings have higher hardness and strength and are rich in SiO2、Al2O3、Fe2O3And chemical components such as CaO, so the utilization of molybdenum tailings is mainly focused on manufacturing building materials, such as cement clinker, heat insulation materials, ceramics (201511031607.7), pervious concrete (201711447355.5) and the like. But to molybdenum tailingsThe application of the hydrophobic modified surface in the aspects of developing cheap hydrophobic admixtures, carriers, anti-wear agents, additives and the like has not been reported in related patents and documents.
Disclosure of Invention
The invention mainly aims at the defects in the background technology and provides a preparation method of hydrophobic molybdenum tailing powder, the method adopts waste molybdenum tailing slag as a main raw material to prepare a hydrophobic product, and the obtained hydrophobic molybdenum tailing powder has the characteristics of high activation degree, high molybdenum tailing utilization rate and the like.
In order to solve the technical problems, the invention adopts the technical scheme that: the preparation method of the hydrophobic molybdenum tailing powder is characterized by comprising the following steps:
step one, carrying out wet ball milling on molybdenum tailing slag to obtain molybdenum tailing powder;
step two, drying the molybdenum tailing powder, adding hydrochloric acid into the dried molybdenum tailing powder, and stirring and washing under a water bath condition to obtain a mixture;
step three, filtering the mixture in the step two, washing and drying the intercepted substance obtained by filtering;
step four, grinding and dispersing the retentate dried in the step three, and then adding NaOH solution, stirring and washing to obtain a mixture;
step five, filtering the mixture obtained in the step four, washing the intercepted substance obtained by filtering, and drying;
adding a dispersing agent into the surfactant solution, and stirring for 20-50 min to obtain a hydrophobic modifier;
step seven, grinding and dispersing the retentate dried in the step five, then adding the grinded and dispersed retentate into the hydrophobic modifier in the step six, and stirring in a water bath to form uniform suspension;
and step eight, filtering the suspension liquid obtained in the step seven, drying the intercepted substance obtained by filtering, grinding by a dry method, and sieving to obtain hydrophobic molybdenum tailing powder.
The preparation method of the hydrophobic molybdenum tailing powder is characterized in that the average particle size of the molybdenum tailing powder in the step one is less than or equal to 10 microns.
The preparation method of the hydrophobic molybdenum tailing powder is characterized in that the average particle size of the molybdenum tailing powder in the step one is 3-5 microns.
The preparation method of the hydrophobic molybdenum tailing powder is characterized in that the concentration of hydrochloric acid in the second step is 9-12 mol/L, and the mass ratio of the molybdenum tailing powder dried in the second step to the hydrochloric acid is 1 (3-5).
The preparation method of the hydrophobic molybdenum tailing powder is characterized in that the drying temperature in the second step is 100-120 ℃; in the second step, the temperature of the water bath is 60-80 ℃, and the stirring and immersion time is 1-5 h.
The preparation method of the hydrophobic molybdenum tailing powder is characterized in that the concentration of the NaOH solution in the fourth step is 4-10 mol/L, the mass ratio of the interception substances ground and dispersed in the fourth step to the NaOH solution is 1 (1-4), and the stirring and immersion washing time in the fourth step is 1-5 hours.
The preparation method of the hydrophobic molybdenum tailing powder is characterized in that the flushing methods in the third step and the fifth step are respectively 3-5 times of repeated flushing by tap water, deionized water or distilled water; the drying temperature in the third step and the drying temperature in the fifth step are both 100-120 ℃.
The preparation method of the hydrophobic molybdenum tailing powder is characterized in that in the sixth step, the mass percentage of the surfactant in the surfactant solution is 1% -10%, the surfactant is methyl hydrogen-containing silicone oil and a silane coupling agent KH570, and the mass ratio of the methyl hydrogen-containing silicone oil to the silane coupling agent KH570 is 1 (0.1-1).
The preparation method of the hydrophobic molybdenum tailing powder is characterized in that the dispersant in the sixth step is dichloromethane, and the amount of the dispersant added in each 100mL of the surfactant solution is 2-4 g.
The preparation method of the hydrophobic molybdenum tailing powder is characterized in that in the seventh step, the amount of the interception after grinding and dispersing is 3 g-7 g added into every 100mL of hydrophobic modifier; and the temperature of water bath stirring in the step seven is 60-100 ℃, and the time is 20-60 min.
The invention has the following advantages:
1. the method adopts the waste molybdenum tailings as the main raw material to prepare the hydrophobic product, belongs to the reutilization of solid waste, meets the requirements of national policies, and has the remarkable characteristics of easily obtained raw materials and low cost.
2. In the preparation method of the hydrophobic molybdenum tailing powder, the acid and the alkali can be recycled, so that the resources are effectively saved; the hydrophobic molybdenum tailing slag is subjected to hydrophobic modification by organically combining the processes of ball milling, impurity removal, modification and the like, so that hydrophobic molybdenum tailing powder with high activation degree and good hydrophobic performance is obtained.
3. The hydrophobic molybdenum tailing powder prepared by the method has the advantages that the activation degree can reach 98%, the molybdenum tailing utilization rate can reach more than 90%, and the hydrophobic molybdenum tailing powder has good performance and extremely high economic and social benefits.
The technical solution of the present invention is further described in detail by examples below.
Drawings
FIG. 1 is a comparison graph of the microscopic morphology of the hydrophobic molybdenum tailing powder of the invention and the molybdenum tailing powder without hydrophobic treatment.
Fig. 2 is a diagram of the hydrophobic effect of the molybdenum tailing powder in example 1 of the present invention.
Fig. 3 is a diagram of the hydrophobic effect of the molybdenum tailing powder in example 2 of the present invention.
Fig. 4 is a diagram of the hydrophobic effect of the molybdenum tailing powder in example 3 of the present invention.
Fig. 5 is a diagram of the hydrophobic effect of the molybdenum tailing powder in example 5 of the present invention.
Detailed Description
Example 1
Step one, carrying out wet ball milling on molybdenum tailing slag to obtain molybdenum tailing powder, wherein the average particle size of the molybdenum tailing powder is 3 microns;
step two, drying the molybdenum tailing powder at the temperature of 100 ℃, adding hydrochloric acid with the concentration of 9mol/L into the dried molybdenum tailing powder, and stirring and washing under the water bath condition to obtain a mixture; the mass ratio of the dried molybdenum tailing powder to the hydrochloric acid is 1: 3; the temperature of the water bath is 60 ℃, and the time is 1 h;
step three, filtering the mixture in the step two, washing the retentate obtained by filtering with tap water for 5 times, and drying again at 100 ℃;
step four, grinding and dispersing the retentate dried in the step three, and then adding a NaOH solution with the concentration of 4mol/L, stirring and washing to obtain a mixture; the mass ratio of the intercepted substances after grinding and dispersion to the NaOH solution is 1:1, and the stirring and immersion washing time is 1 h;
step five, filtering the mixture in the step four, washing the retentate obtained by filtering with tap water for 3 times, and drying again at the temperature of 100 ℃;
adding a dispersing agent into the surfactant solution, and stirring for 20min to obtain a hydrophobic modifier; the mass percentage of the surfactant in the surfactant solution is 1 percent, the surfactant is methyl hydrogen-containing silicone oil and a silane coupling agent KH570, and the mass ratio of the methyl hydrogen-containing silicone oil to the silane coupling agent KH570 is 1: 0.1;
the dispersing agent is dichloromethane, and the amount of the dispersing agent added in each 100mL of the surfactant solution is 2 g;
step seven, grinding and dispersing the dried retentate obtained in the step five, then adding 3g of the ground and dispersed retentate into 100mL of the hydrophobic modifier obtained in the step six, and stirring in a water bath to form uniform suspension; stirring in water bath at 60 deg.C for 20 min;
and step eight, filtering the suspension in the step seven, drying the filtered retentate, grinding the retentate by a dry method, and sieving the retentate to obtain hydrophobic molybdenum tailing powder with the particle size of less than or equal to 10 microns.
Fig. 1 is a comparison graph of appearance and appearance of the molybdenum tailing powder of the embodiment before and after water repellent, and it can be seen from the graph that the dispersibility of the modified powder is improved, the surface of the powder is not smooth, and the powder has a coating substance.
Example 2
Step one, carrying out wet ball milling on molybdenum tailing slag to obtain molybdenum tailing powder, wherein the average particle size of the molybdenum tailing powder is 4 microns;
step two, drying the molybdenum tailing powder at the temperature of 110 ℃, adding hydrochloric acid with the concentration of 10mol/L into the dried molybdenum tailing powder, and stirring and washing under the water bath condition to obtain a mixture; the mass ratio of the dried molybdenum tailing powder to the hydrochloric acid is 1: 5; the temperature of the water bath is 70 ℃, and the time is 2 hours;
step three, filtering the mixture in the step two, washing the intercepted substance obtained by filtering with deionized water for 4 times, and drying again at 110 ℃;
step four, grinding and dispersing the retentate dried in the step three, and then adding a NaOH solution with the concentration of 6mol/L, stirring and washing to obtain a mixture; the mass ratio of the intercepted substances after grinding and dispersion to the NaOH solution is 1:4, and the stirring and immersion washing time is 2 hours;
step five, filtering the mixture obtained in the step four, washing the intercepted substance obtained by filtering with deionized water for 4 times, and drying again at the temperature of 110 ℃;
adding a dispersing agent into the surfactant solution, and stirring for 30min to obtain a hydrophobic modifier; the mass percentage of the surfactant in the surfactant solution is 3%, the surfactant is methyl hydrogen-containing silicone oil and a silane coupling agent KH570, and the mass ratio of the methyl hydrogen-containing silicone oil to the silane coupling agent KH570 is 1: 0.3;
the dispersing agent is dichloromethane, and the amount of the dispersing agent added in each 100mL of the surfactant solution is 3 g;
step seven, grinding and dispersing the dried retentate obtained in the step five, then adding 4g of the grinded and dispersed retentate into 100mL of the hydrophobic modifier obtained in the step six, and stirring in a water bath to form uniform suspension; stirring in water bath at 70 deg.C for 30 min;
and step eight, filtering the suspension in the step seven, drying the filtered retentate, grinding the retentate by a dry method, and sieving the retentate to obtain hydrophobic molybdenum tailing powder with the particle size of less than or equal to 10 microns.
Example 3
Step one, carrying out wet ball milling on molybdenum tailing slag to obtain molybdenum tailing powder, wherein the average particle size of the molybdenum tailing powder is 5 microns;
step two, drying the molybdenum tailing powder at 120 ℃, adding hydrochloric acid with the concentration of 11mol/L into the dried molybdenum tailing powder, and stirring and washing under the water bath condition to obtain a mixture; the mass ratio of the dried molybdenum tailing powder to the hydrochloric acid is 1: 4; the temperature of the water bath is 80 ℃, and the time is 3 hours;
step three, filtering the mixture in the step two, washing the retentate obtained by filtering with distilled water for 5 times, and drying again at 120 ℃;
step four, grinding and dispersing the retentate dried in the step three, and then adding a NaOH solution with the concentration of 8mol/L, stirring and washing to obtain a mixture; the mass ratio of the intercepted substances after grinding and dispersion to the NaOH solution is 1:2, and the stirring and immersion washing time is 3 hours;
step five, filtering the mixture in the step four, washing the retentate obtained by filtering with distilled water for 5 times, and drying again at 120 ℃;
adding a dispersing agent into the surfactant solution, and stirring for 40min to obtain a hydrophobic modifier; the mass percentage of the surfactant in the surfactant solution is 5%, the surfactant is methyl hydrogen-containing silicone oil and a silane coupling agent KH570, and the mass ratio of the methyl hydrogen-containing silicone oil to the silane coupling agent KH570 is 1: 0.5;
the dispersing agent is dichloromethane, and the amount of the dispersing agent added in each 100mL of the surfactant solution is 4 g;
step seven, grinding and dispersing the dried retentate obtained in the step five, then adding 5g of the ground and dispersed retentate into 100mL of the hydrophobic modifier obtained in the step six, and stirring in a water bath to form uniform suspension; stirring in water bath at 80 deg.C for 40 min;
and step eight, filtering the suspension in the step seven, drying the filtered retentate, grinding the retentate by a dry method, and sieving the retentate to obtain hydrophobic molybdenum tailing powder with the particle size of less than or equal to 10 microns.
Example 4
Step one, carrying out wet ball milling on molybdenum tailing slag to obtain molybdenum tailing powder, wherein the average particle size of the molybdenum tailing powder is 8 microns;
step two, drying the molybdenum tailing powder at 120 ℃, adding hydrochloric acid with the concentration of 12mol/L into the dried molybdenum tailing powder, and stirring and washing under the water bath condition to obtain a mixture; the mass ratio of the dried molybdenum tailing powder to the hydrochloric acid is 1: 3; the temperature of the water bath is 80 ℃, and the time is 4 hours;
step three, filtering the mixture in the step two, washing the retentate obtained by filtering with tap water for 3 times, and drying again at 120 ℃;
step four, grinding and dispersing the retentate dried in the step three, and then adding a NaOH solution with the concentration of 10mol/L, stirring and washing to obtain a mixture; the mass ratio of the intercepted substances after grinding and dispersion to the NaOH solution is 1:1, and the stirring and immersion washing time is 4 hours;
step five, filtering the mixture in the step four, washing the retentate obtained by filtering with tap water for 5 times, and drying again at 120 ℃;
adding a dispersing agent into the surfactant solution, and stirring for 50min to obtain a hydrophobic modifier; the mass percentage of the surfactant in the surfactant solution is 7%, the surfactant is methyl hydrogen-containing silicone oil and a silane coupling agent KH570, and the mass ratio of the methyl hydrogen-containing silicone oil to the silane coupling agent KH570 is 1: 0.7;
the dispersing agent is dichloromethane, and the amount of the dispersing agent added in each 100mL of the surfactant solution is 4 g;
step seven, grinding and dispersing the dried retentate obtained in the step five, then adding 7g of the ground and dispersed retentate into 100mL of the hydrophobic modifier obtained in the step six, and stirring in a water bath to form uniform suspension; stirring in water bath at 80 deg.C for 60 min;
and step eight, filtering the suspension in the step seven, drying the filtered retentate, grinding the retentate by a dry method, and sieving the retentate to obtain hydrophobic molybdenum tailing powder with the particle size of less than or equal to 10 microns.
Example 5
Step one, carrying out wet ball milling on molybdenum tailing slag to obtain molybdenum tailing powder, wherein the average particle size of the molybdenum tailing powder is 10 microns;
step two, drying the molybdenum tailing powder at 120 ℃, adding hydrochloric acid with the concentration of 12mol/L into the dried molybdenum tailing powder, and stirring and washing under the water bath condition to obtain a mixture; the mass ratio of the dried molybdenum tailing powder to the hydrochloric acid is 1: 3; the temperature of the water bath is 80 ℃, the time is 4h,
step three, filtering the mixture obtained in the step two, washing the retentate obtained by filtering with distilled water for 5 times, and drying again at 120 ℃ to obtain dried molybdenum tailing powder;
step four, grinding and dispersing the retentate dried in the step three, then adding a NaOH solution with the concentration of 10mol/L, stirring and washing to obtain a mixture; the mass ratio of the intercepted substances after grinding and dispersion to the NaOH solution is 1:1, and the stirring and immersion washing time is 5 hours;
step five, filtering the mixture in the step four, washing the retentate obtained by filtering with distilled water for 5 times, and drying at 120 ℃;
adding a dispersing agent into the surfactant solution, and stirring for 50min to obtain a hydrophobic modifier; the mass percentage of the surfactant in the surfactant solution is 10%, the surfactant is methyl hydrogen-containing silicone oil and a silane coupling agent KH570, and the mass ratio of the methyl hydrogen-containing silicone oil to the silane coupling agent KH570 is 1: 1;
the dispersing agent is dichloromethane, and the amount of the dispersing agent added in each 100mL of the surfactant solution is 4 g;
step seven, grinding and dispersing the dried retentate obtained in the step five, then adding 7g of the ground and dispersed retentate into 100mL of the hydrophobic modifier obtained in the step six, and stirring in a water bath to form uniform suspension; stirring in water bath at 100 deg.C for 60 min;
and step eight, filtering the suspension in the step seven, drying the filtered retentate, grinding the retentate by a dry method, and sieving the retentate to obtain hydrophobic molybdenum tailing powder with the particle size of less than or equal to 10 microns.
Weighing the hydrophobic molybdenum tailing powder obtained in the embodiment 1-5, adding the powder into a beaker filled with distilled water, magnetically stirring for 20min, standing for 24h, filtering a sample precipitated at the bottom of the beaker, drying a retentate obtained by filtering, and weighing;
the degree of activation H is calculated as:
wherein, W1Weighing the mass g of the hydrophobic molybdenum tailing powder;
W2mass of the dried retentate, g;
TABLE 1 hydrophobic Properties of molybdenum tailings under different process conditions
As can be seen from table 1, the activation degree of the hydrophobic molybdenum tailing powder is as high as approximately 98%, and with reference to fig. 2 to 5, the water drops do not wet and stably exist on the surface of the hydrophobic molybdenum tailing powder, and the water drops are spherical in the example 2 (fig. 3) and the example 3 (fig. 4), which indicates that the hydrophobic molybdenum tailing powder has good hydrophobic property.
Example 6
The hydrophobic molybdenum tailing powder in the embodiment 2 and the embodiment 3 is taken and respectively mixed with ammonium phosphate (90% of particle size is less than 20 microns) to prepare the dry powder extinguishing agent, the mass percentage of the hydrophobic molybdenum tailing powder in the dry powder extinguishing agent is 5% -7%, and the water repellency, the water content and the moisture absorption rate of the prepared dry powder extinguishing agent are detected according to the industrial standard GA 578 and 2005 ultrafine dry powder extinguishing agent. The display results of water repellency are 'no obvious water absorption and no agglomeration', and meet the standard requirements; the water content detection results are respectively 0.223% (embodiment 2) and 0.214% (embodiment 3), and the standard requirements are met; the results of moisture absorption rate measurements were 2.78% (example 2) and 2.42% (example 3), respectively, and met the standard requirements.
The detection result of the relevant performance of the superfine ammonium phosphate salt dry powder extinguishing agent prepared from the white carbon black on the market at present shows that the height of a hydrophobic boss generated by the ammonium phosphate salt dry powder extinguishing agent prepared from the hydrophobic molybdenum tailing powder is obviously higher than that of the boss of the superfine dry powder extinguishing agent prepared from the hydrophobic white carbon black on the market, which shows that the product can improve the water repellency and the moisture absorption and caking resistance of the superfine dry powder extinguishing agent, and the raw material used by the product is mine waste slag, so that the product has higher market advantage with low cost.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (7)
1. The preparation method of the hydrophobic molybdenum tailing powder is characterized by comprising the following steps:
step one, carrying out wet ball milling on molybdenum tailing slag to obtain molybdenum tailing powder;
step two, drying the molybdenum tailing powder in the step one, adding hydrochloric acid into the dried molybdenum tailing powder, and stirring and washing under a water bath condition to obtain a mixture; the concentration of the hydrochloric acid is 9-12 mol/L, and the mass ratio of the dried molybdenum tailing powder to the hydrochloric acid is 1 (3-5);
step three, filtering the mixture in the step two, washing and drying the intercepted substance obtained by filtering;
step four, grinding and dispersing the retentate dried in the step three, and then adding NaOH solution, stirring and washing to obtain a mixture;
step five, filtering the mixture obtained in the step four, washing the intercepted substance obtained by filtering, and drying;
adding a dispersing agent into the surfactant solution, and stirring for 20-50 min to obtain a hydrophobic modifier; the mass percentage of the surfactant in the surfactant solution is 1-10%, the surfactant is methyl hydrogen-containing silicone oil and a silane coupling agent KH570, and the mass ratio of the methyl hydrogen-containing silicone oil to the silane coupling agent KH570 is 1 (0.1-1); the dispersant is dichloromethane, and the amount of the dispersant added in each 100mL of the surfactant solution is 2 g-4 g;
step seven, grinding and dispersing the retentate dried in the step five, then adding the grinded and dispersed retentate into the hydrophobic modifier in the step six, and stirring in a water bath to form uniform suspension;
and step eight, filtering the suspension liquid obtained in the step seven, drying the intercepted substance obtained by filtering, grinding by a dry method, and sieving to obtain hydrophobic molybdenum tailing powder.
2. The method for preparing hydrophobic molybdenum tailing powder according to claim 1, wherein the average particle size of the molybdenum tailing powder in the first step is less than or equal to 10 μm.
3. The method for preparing hydrophobic molybdenum tailing powder according to claim 2, wherein the average particle size of the molybdenum tailing powder in the first step is 3-5 μm.
4. The method for preparing the hydrophobic molybdenum tailing powder according to claim 1, wherein the temperature of the drying treatment in the second step is 100-120 ℃; in the second step, the temperature of the water bath is 60-80 ℃, and the stirring and immersion time is 1-5 h.
5. The preparation method of the hydrophobic molybdenum tailing powder according to claim 1, wherein the concentration of the NaOH solution in the fourth step is 4-10 mol/L, the mass ratio of the interception substance ground and dispersed in the fourth step to the NaOH solution is 1 (1-4), and the stirring and soaking time in the fourth step is 1-5 hours.
6. The method for preparing the hydrophobic molybdenum tailing powder according to claim 1, wherein the flushing methods in the third step and the fifth step are repeated flushing for 3 to 5 times by using tap water, deionized water or distilled water; the drying temperature in the third step and the drying temperature in the fifth step are both 100-120 ℃.
7. The method for preparing hydrophobic molybdenum tailing powder according to claim 1, wherein the amount of the retentate after grinding and dispersing added into every 100mL of hydrophobic modifier in the seventh step is 3 g-7 g; and the temperature of water bath stirring in the step seven is 60-100 ℃, and the time is 20-60 min.
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