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CN-121988460-A - Flotation collector for scheelite and preparation method thereof

CN121988460ACN 121988460 ACN121988460 ACN 121988460ACN-121988460-A

Abstract

The invention relates to the technical field of mineral flotation, in particular to a flotation collector for scheelite and a preparation method thereof. The flotation collector for scheelite comprises, by weight, 40-60 parts of a compound A, 10-20 parts of sodium oleate, 5-8 parts of thiadiazole acid and 1-5 parts of an emulsifier. The flotation collector for scheelite can improve concentrate yield, grade and recovery rate.

Inventors

  • KONG LINGJIAN
  • ZHANG FANFAN
  • LI BOTAO
  • ZHAO YANZHAO
  • CHEN QINGAN

Assignees

  • 栾川县长青钨钼有限责任公司
  • 郑州大学

Dates

Publication Date
20260508
Application Date
20260408

Claims (9)

  1. 1. The flotation collector for scheelite is characterized by comprising, by weight, 40-60 parts of a compound A, 10-20 parts of sodium oleate, 5-8 parts of thiadiazole acid and 1-5 parts of an emulsifier; The structural formula of the compound A is as follows: 。
  2. 2. The flotation collector for scheelite according to claim 1, wherein the process for preparing the compound a is as follows: (1) Under the protection of inert gas, adding 5' -cytidine acid into anhydrous pyridine, adding dicyclohexylcarbodiimide and isobutanol, and purifying after reaction to obtain an intermediate 1; The structural formula of the intermediate 1 is as follows: (2) Under the protection of inert gas, adding the intermediate 1 into anhydrous pyridine, adding trimethylchlorosilane for hydroxyl protection reaction, then adding lauric anhydride for acylation reaction, removing protecting groups after the reaction is finished, and purifying to obtain the compound A.
  3. 3. The flotation collector for scheelite according to claim 2, wherein the molar ratio of 5' -cytidine acid, isobutanol and dicyclohexylcarbodiimide in step (1) is 1 (3-4): 4-5, the reaction temperature is 40-45 ℃ and the reaction time is 18-24 hours.
  4. 4. The flotation collector for scheelite according to claim 2, wherein the dosage ratio of the intermediate 1, the trimethylchlorosilane and the lauric anhydride in the step (2) is 1mmol (0.6-1.1) mL (1-1.2) mmol, the temperature of the hydroxyl protection reaction is 0-5 ℃ and the time is 1-1.5h.
  5. 5. The flotation collector for scheelite according to claim 2, wherein the acylation reaction in step (2) is carried out by stirring for 2-3 hours at-10 to-5 ℃, then heating to 20-25 ℃ and stirring for 1-2 hours.
  6. 6. The flotation collector for scheelite according to claim 1, wherein the emulsifier is tween 60 or polyoxyethylene ether.
  7. 7. A method of preparing a flotation collector for scheelite according to any one of claims 1 to 6, comprising the steps of: and (3) mixing the compound A, sodium oleate, thiodiacid and an emulsifier according to the parts by weight, adding deionized water to obtain a mixed solution, regulating the pH value, and stirring.
  8. 8. The method for producing a collector for scheelite flotation according to claim 7, wherein the total mass fraction of all the raw materials in the mixed solution is 8 to 15%, and the pH is adjusted to 8 to 9.
  9. 9. The method for preparing a flotation collector for scheelite according to claim 7, wherein the stirring temperature is 40-50 ℃, the speed is 500-1000r/min, and the time is 20-50min.

Description

Flotation collector for scheelite and preparation method thereof Technical Field The invention relates to the technical field of mineral flotation, in particular to a flotation collector for scheelite and a preparation method thereof. Background Tungsten is an important strategic metal, has the characteristics of high density, low vapor pressure, high melting point and low thermal expansion coefficient, is known as industrial teeth, and is commonly used for manufacturing alloys, catalysts, semiconductors, electronic and electric products and the like. Tungsten ore resources mainly comprise scheelite and scheelite, and along with the increasing reduction of easily-selected scheelite resources, the recycling of scheelite resources is increasingly receiving attention. Flotation is the main method for separating and purifying scheelite. However, WO 42-、F- and CO 32- generated by dissolving scheelite and calcium-containing gangue minerals such as fluorite, calcite, apatite and the like in ore pulp can generate chemical reaction on the surfaces of the minerals, so that the surfaces of the minerals are mutually converted, the physical and chemical properties of the surfaces are similar, and further, the flotation separation of the scheelite and the calcium-containing gangue minerals is difficult. The traditional fatty acid collector (oleic acid, oxidized paraffin soap and the like) has poor selectivity and is easy to combine with calcium-containing gangue, other alternative collectors such as benzohydroxamic acid have the problem of poor collecting capacity, and extremely toxic lead nitrate is required to be activated, so that the separation efficiency cannot be effectively improved. There is a need to develop a collector with a high recovery capacity and high selectivity for scheelite flotation to achieve efficient flotation separation between scheelite and calcium-containing gangue minerals. Disclosure of Invention In order to overcome the defects of the prior art, one of the purposes of the invention is to provide a flotation collector for scheelite, which can improve concentrate yield, grade and recovery rate. The second purpose of the invention is to provide a preparation method of the flotation collector for scheelite, which is simple to operate. One of the purposes of the invention is realized by adopting the following technical scheme: The flotation collector for scheelite comprises, by weight, 40-60 parts of a compound A, 10-20 parts of sodium oleate, 5-8 parts of thiadiazole acid and 1-5 parts of an emulsifier; The structural formula of the compound A is as follows: 。 Further, the preparation process of the compound A is as follows: (1) Under the protection of inert gas, adding 5' -cytidine acid into anhydrous pyridine, adding dicyclohexylcarbodiimide and isobutanol, and purifying after reaction to obtain an intermediate 1; The structural formula of the intermediate 1 is as follows: (2) Under the protection of inert gas, adding the intermediate 1 into anhydrous pyridine, adding trimethylchlorosilane for hydroxyl protection reaction, then adding lauric anhydride for acylation reaction, removing protecting groups after the reaction is finished, and purifying to obtain the compound A. The preparation process of the compound A comprises the steps of carrying out esterification reaction on 5 '-cytidine acid and isobutanol under the action of Dicyclohexylcarbodiimide (DCC) to form an intermediate 1 containing a phosphate bond, protecting the ortho-dihydroxyl (from 5' -cytidine acid) of a furan ring of the intermediate 1 by using trimethylchlorosilane, carrying out acylation reaction on the ortho-dihydroxyl and lauric anhydride under the heating condition, deprotecting the hydroxyl by using concentrated ammonia water after the reaction is finished, and finally purifying to obtain the compound A which is used as a main collector for scheelite flotation. Further, in the step (1), the molar ratio of the 5' -cytidine acid, the isobutanol and the dicyclohexylcarbodiimide is 1 (3-4): 4-5, the reaction temperature is 40-45 ℃ and the reaction time is 18-24 hours. Further, in the step (2), the dosage ratio of the intermediate 1, the trimethylchlorosilane and the lauric anhydride is 1mmol (0.6-1.1) mL (1-1.2) mmol, the temperature of the hydroxyl protection reaction is 0-5 ℃ and the time is 1-1.5h. Further, in the step (2), the acylation reaction is carried out by stirring for 2-3h at-10 to-5 ℃, then heating to 20-25 ℃ and stirring for 1-2h. Further, the emulsifier is tween 60 or polyoxyethylene ether. The second purpose of the invention is realized by adopting the following technical scheme: the preparation method of the flotation collector for scheelite comprises the following steps: and (3) mixing the compound A, sodium oleate, thiodiacid and an emulsifier according to the parts by weight, adding deionized water to obtain a mixed solution, regulating the pH value, and stirring. Further, the total mass fraction of all