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CN-121990902-A - Preparation process of composite collector for low-temperature spodumene floatation

CN121990902ACN 121990902 ACN121990902 ACN 121990902ACN-121990902-A

Abstract

The invention relates to the technical field of mineral processing, and discloses a preparation process of a composite collector for low-temperature spodumene flotation, which comprises, by weight, 20% -30% of oxidized paraffin soap, 3% -8% of dialkylphosphinic acid, 8% -12% of fatty acid methyl ester ethoxylate, 5% -10% of kerosene, 15% -20% of propylene glycol, 1% -3% of 1-butyl-3-methylimidazole hexafluorophosphate, 0.1% -0.5% of potassium sorbate, 3% -5% of methyl isobutyl carbinol, 10% -15% of triethanolamine, and the steps of dewatering and pre-activating the oxidized paraffin soap, the dialkylphosphinic acid and the triethanolamine, sequentially mixing the oxidized paraffin soap, the dialkylphosphinic acid and the triethanolamine in a mixing stage A, a stage B and a stage C, finally detecting the pH value, the viscosity, the low-temperature stability and the effective activity content, and obtaining a finished product through nitrogen protection packaging.

Inventors

  • Liao Qiuguang
  • XIE FANG
  • LIU JIANPING
  • ZHANG CHI
  • LI WENJUAN
  • LIAO YANG

Assignees

  • 宜春学院

Dates

Publication Date
20260508
Application Date
20260113

Claims (10)

  1. 1. The preparation process of the composite collector for low-temperature spodumene floatation is characterized by comprising the following steps of: Preparing oxidized paraffin soap, dialkyl phosphinic acid, fatty acid methyl ester ethoxylate, kerosene, propylene glycol, 1-butyl-3-methylimidazole hexafluorophosphate, potassium sorbate, methyl isobutyl carbinol and triethanolamine according to the weight ratio of the formula; step two, pretreatment, namely respectively carrying out dehydration and pre-activation pretreatment on the prepared oxidized paraffin soap, dialkyl phosphinic acid and triethanolamine; step three, a mixing stage A is that pretreated oxidized paraffin soap, dialkyl phosphinic acid and triethanolamine are added into a reaction kettle, and preliminary mixing and saponification reaction are carried out; Step four, mixing the product of the step A, namely sequentially adding fatty acid methyl ester ethoxylate, kerosene, propylene glycol and 1-butyl-3-methylimidazole hexafluorophosphate into the product of the step B, and emulsifying and dispersing; Step five, a mixing stage C, namely cooling the system to 25-30 ℃, adding methyl isobutyl carbinol and potassium sorbate, and carrying out final tempering homogenization; and step six, quality detection and packaging, namely detecting pH value, viscosity, low-temperature stability and effective activity content, and packaging qualified products by nitrogen protection to obtain a finished product of the composite collector.
  2. 2. The preparation process of the composite collector for low-temperature spodumene flotation according to claim 1, wherein the composite collector comprises, by weight, 20% -30% of oxidized paraffin soap, 3% -8% of dialkylphosphinic acid, 8% -12% of fatty acid methyl ester ethoxylate, 5% -10% of kerosene, 15% -20% of propylene glycol, 1% -3% of 1-butyl-3-methylimidazole hexafluorophosphate, 0.1% -0.5% of potassium sorbate, 3% -5% of methyl isobutyl carbinol and 10% -15% of triethanolamine.
  3. 3. The process for preparing the composite collector for low-temperature spodumene floatation as claimed in claim 1, wherein the oxidized paraffin soap is prepared by air oxidation of paraffin and saponification reaction with sodium hydroxide, and has the chemical formula: (1) Oxidation reaction: in the formula, Is the mixture of the alkanes in the raw material paraffin, Is the oxygen in the air, and the oxygen in the air is the oxygen in the air, Is fatty acid generated by oxidation; (2) Saponification reaction: in the formula, In order to oxidize the product fatty acid, In order to obtain the saponification reagent, In order to produce the end product oxidized paraffin soap, Is saponification reaction water.
  4. 4. The preparation process of the composite collector for low-temperature spodumene floatation, which is characterized by comprising the following step of drying oxidized paraffin soap at 55-60 ℃ and a vacuum degree of-0.09 to-0.08 MPa for 2-3 hours to ensure that the moisture content of the oxidized paraffin soap is less than or equal to 0.5 percent.
  5. 5. The preparation process of the composite collector for low-temperature spodumene flotation according to claim 1, wherein the pretreatment conditions in the second step are that dialkylphosphinic acid is dissolved in absolute ethyl alcohol with the concentration of more than or equal to 99%, and then is subjected to water bath dissolution at 70-75 ℃ and crystallization at low temperature of 0-4 ℃ for 6-8 hours for purification, and after vacuum filtration and washing of crystals with the same-concentration absolute ethyl alcohol precooled to 0-4 ℃ for 2-3 times, the crystals are dried for 2-3 hours at 55-60 ℃ and vacuum degree of-0.09-0.08 MPa, so that white dialkylphosphinic acid crystalline solid with the purity of more than or equal to 98% is obtained.
  6. 6. The preparation process of the composite collector for low-temperature spodumene flotation according to claim 1, wherein the pretreatment condition in the second step is that triethanolamine is subjected to dynamic dehydration treatment by a 4A type molecular sieve for 36-48 hours, so that the moisture content of the triethanolamine is less than or equal to 0.2%.
  7. 7. The process for preparing the composite collector for low-temperature spodumene floatation according to claim 1, wherein the three-stage A mixing condition comprises the following steps of reacting for 40-50 minutes under the stirring condition of 45-50 ℃ and 200-300rpm, converting a system from turbidity into uniform light yellow transparent liquid, and the saponification reaction chemical formula in the process is as follows: in the formula, Indicating the long chain fatty acid component contained in the oxidized paraffin mixture, wherein Is mainly of carbon number Is used for the preparation of a polymer, Represents a combination of triethanolamine and triethanolamine, Represents the triethanolamine fatty acid salt generated by the reaction, Is produced as a trace by-product.
  8. 8. The process for preparing the composite collector for low-temperature spodumene floatation according to claim 1, wherein the four-stage B mixing condition is that the temperature is maintained at 40-45 ℃, the rotating speed is gradually increased to 800-1000rpm in a staged gradient speed increasing mode, and shearing and emulsifying are carried out for 50-60 minutes to form stable oil-in-water emulsion.
  9. 9. The process for preparing the composite collector for low-temperature spodumene floatation according to claim 1, wherein the mixing condition of the step five is that the mixture is stirred at the speed of 300-400rpm at 22-25 ℃ for 20-25 minutes, so that the amber semitransparent liquid with uniform fluidity is obtained.
  10. 10. The process for preparing the composite collector for low-temperature spodumene floatation according to claim 1, wherein the composite collector is used for selectively collecting spodumene minerals in low-temperature spodumene floatation at a temperature of 5-15 ℃ in a low-temperature ore pulp environment.

Description

Preparation process of composite collector for low-temperature spodumene floatation Technical Field The invention relates to the technical field of mineral processing, in particular to a preparation process of a composite collector for low-temperature spodumene floatation. Background Spodumene is used as one of main minerals for extracting lithium resources, and efficient separation of spodumene is a key link of a lithium battery industry chain. Flotation is the core method for concentrating spodumene, wherein anionic collectors (such as oxidized paraffin soaps) are widely used. However, under the conditions of high altitude, high latitude or low temperature in winter, the conventional collector represented by oxidized paraffin soap (mainly comprising fatty acid sodium salt) has obvious defects of rapid reduction of sodium soap solubility and dispersibility, easy crystallization and precipitation, effective ingredient loss and reduction of collecting activity, and meanwhile, molecular diffusion is slowed down at low temperature, adsorption kinetics is deteriorated, and selective collecting capacity of spodumene is reduced. To solve this problem, the prior art relies on external heating of the pulp or the use of a large amount of solvents, which not only has high energy consumption and high cost, but also may introduce environmental protection and safety problems. Some researches try to compound various medicaments to improve low-temperature performance, but often neglect low-temperature compatibility and a synergistic mechanism among components, so that the formula is complex, the effect is unstable, and high selectivity, high recovery rate and wide ore adaptability are difficult to be achieved. Disclosure of Invention (One) solving the technical problems Aiming at the defects of the prior art, the invention provides a preparation process of a composite collector for low-temperature spodumene flotation, which has the advantages of good solubility and dispersibility at low temperature, high adsorption selectivity, energy conservation, high efficiency and strong universality, and solves the problems of low activity, poor selectivity, dependence on external heating and high energy consumption of the traditional collector in a low-temperature environment. (II) technical scheme In order to achieve the purpose, the invention provides the following technical scheme that the preparation process of the composite collector for low-temperature spodumene floatation comprises the following steps: Preparing oxidized paraffin soap, dialkyl phosphinic acid, fatty acid methyl ester ethoxylate, kerosene, propylene glycol, 1-butyl-3-methylimidazole hexafluorophosphate, potassium sorbate, methyl isobutyl carbinol and triethanolamine according to the weight ratio of the formula; step two, pretreatment, namely respectively carrying out dehydration and pre-activation pretreatment on the prepared oxidized paraffin soap, dialkyl phosphinic acid and triethanolamine; step three, a mixing stage A is that pretreated oxidized paraffin soap, dialkyl phosphinic acid and triethanolamine are added into a reaction kettle, and preliminary mixing and saponification reaction are carried out; Step four, mixing the product of the step A, namely sequentially adding fatty acid methyl ester ethoxylate, kerosene, propylene glycol and 1-butyl-3-methylimidazole hexafluorophosphate into the product of the step B, and emulsifying and dispersing; Step five, a mixing stage C, namely cooling the system to 25-30 ℃, adding methyl isobutyl carbinol and potassium sorbate, and carrying out final tempering homogenization; and step six, quality detection and packaging, namely detecting pH value, viscosity, low-temperature stability and effective activity content, and packaging qualified products by nitrogen protection to obtain a finished product of the composite collector. Preferably, the composite collector in the first step comprises, by weight, 20% -30% of oxidized paraffin soap, 3% -8% of dialkyl phosphinic acid, 8% -12% of fatty acid methyl ester ethoxylate, 5% -10% of kerosene, 15% -20% of propylene glycol, 1% -3% of 1-butyl-3-methylimidazole hexafluorophosphate, 0.1% -0.5% of potassium sorbate, 3% -5% of methyl isobutyl carbinol and 10% -15% of triethanolamine. Preferably, the oxidized paraffin soap is prepared by performing saponification reaction on paraffin after air oxidation and sodium hydroxide, and has a chemical formula as follows: (1) Oxidation reaction: in the formula, Is the mixture of the alkanes in the raw material paraffin,Is the oxygen in the air, and the oxygen in the air is the oxygen in the air,Is fatty acid generated by oxidation; (2) Saponification reaction: in the formula, In order to oxidize the product fatty acid,In order to obtain the saponification reagent,In order to produce the end product oxidized paraffin soap,Is saponification reaction water. Preferably, the pretreatment condition of the second step is that oxidized paraffin s