CN-119715433-B - Quantitative test method for adsorption capacity of benzyl ammonium chloride collector on mineral surface in flotation process

CN119715433BCN 119715433 BCN119715433 BCN 119715433BCN-119715433-B

Abstract

The invention relates to a quantitative test method for adsorption capacity of a benzyl ammonium chloride collector on the surface of a mineral in a flotation process. The testing method provided by the invention avoids photometric measurement errors caused by dissolution of metal ions and anions such as Ca 2+ 、F ‑ and the like from minerals, can detect trace and trace components simultaneously, widens the detection range, avoids operation errors caused by dilution or concentration steps in the detection process of the collecting agent, does not need to introduce additional agents such as an extracting agent and the like, avoids adsorption amount calculation errors caused by incomplete extraction, and has the advantages of simplicity and convenience in operation, high analysis speed, good accuracy and the like.

Inventors

XU YINXIANG
TONG ZHENG
LI FANG
SUN HUALIN
Qiu Nana
GONG PIYU
ZHU MENGYA
FENG XIN
YANG CHAO

Assignees

中国科学院过程工程研究所
宜都兴发化工有限公司

Dates

Publication Date: 20260512
Application Date: 20241220

Claims (8)

1. The quantitative test method for the adsorption capacity of the benzyl ammonium chloride collector on the mineral surface in the flotation process is characterized by comprising the following steps of: mixing minerals to prepare ore pulp, stirring, and performing solid-liquid separation to obtain clear liquid as background solution for ultraviolet detection, wherein the solid-liquid separation is performed by adopting a water-based filter membrane with a membrane pore diameter of 0.1-1 μm; after the ore pulp is mixed with a benzyl ammonium chloride collector, carrying out solid-liquid separation, and taking clear liquid as a sample to be detected; The step of establishing a standard curve for the trace and trace benzyl ammonium chloride collectors includes selecting a suitable absorption wavelength as the ultraviolet detection wavelength for the trace and trace benzyl ammonium chloride collectors; the ultraviolet detection wavelength of the trace benzyl ammonium chloride collector is 200-220nm, and the ultraviolet detection wavelength of the trace benzyl ammonium chloride collector is 185-200nm; Respectively carrying out photometry on the background solution detected by ultraviolet and the sample to be detected by adopting an ultraviolet-visible spectrophotometer, and determining the content of the benzyl ammonium chloride collector in the sample to be detected according to the standard curve of the established trace and trace benzyl ammonium chloride collectors; And calculating the adsorption quantity of the benzyl ammonium chloride collector on the mineral surface through the difference value between the initial concentration of the benzyl ammonium chloride collector and the residual concentration in the sample to be detected.
2. The method of claim 1, wherein the agitating is based on sufficient dissolution of free ions from the mineral surface into the body of water to reach a dissolution equilibrium.
3. The method of claim 1, wherein the concentration of the benzyl ammonium chloride collector after mixing with the pulp is 10 -6 -10 -3 g/mL.
4. The method of claim 1, wherein the mixing is based on gradual adsorption of the benzyl ammonium chloride collector onto the mineral surface to reach adsorption equilibrium.
5. The method of claim 1, wherein the step of establishing a standard curve for trace and trace amounts of benzyl ammonium chloride collectors comprises: Preparing a trace and trace benzyl ammonium chloride collector standard solution, and performing spectrum scanning on the trace and trace benzyl ammonium chloride collector standard solution in a wavelength range of 185-800 nm by using an ultraviolet-visible spectrophotometer and ultrapure water as a background; and selecting proper absorption wavelength as ultraviolet detection wavelength of the trace and trace benzyl ammonium chloride collecting agent, fixing different detection wavelengths to respectively carry out photometry of the trace and trace solutions, establishing the relationship between the concentration and absorbance of the trace and trace benzyl ammonium chloride solution, and drawing a standard curve.
6. The method of claim 5, wherein the concentration of the standard solution of the trace benzyl ammonium chloride collector is 5-100ppm and the concentration of the standard solution of the trace benzyl ammonium chloride collector is 0.1-5ppm.
7. The method according to claim 1, wherein the calculation formula for calculating the adsorption amount of the mineral surface is: ; Wherein Γ is adsorption capacity, kg/m 2 ;c m0 and c m1 are initial concentration and residual concentration of benzyl ammonium chloride collector, g/mL respectively, V is volume of solution, mL, m is mass of mineral sample, g, S is specific surface area of pure mineral, and m 2 /Kg.
8. The method according to claim 1, characterized in that it comprises the steps of: after mineral is prepared into ore pulp, stirring is carried out to fully dissolve free ions on the surface of the mineral into water, after the dissolution balance is achieved, a water system filter membrane with the membrane aperture of 0.1-1 mu m is adopted for solid-liquid separation, and clear liquid is taken as background solution for ultraviolet detection; The ore pulp is mixed with a benzyl ammonium chloride collector, the benzyl ammonium chloride collector is gradually adsorbed on the surface of a mineral, after the adsorption balance is achieved, a water-based filter membrane with the membrane aperture of 0.1-1 mu m is adopted for solid-liquid separation, clear liquid is taken as a solution to be detected, and the concentration of the benzyl ammonium chloride collector after being mixed with the ore pulp is 10 -6 -10 -3 g/mL; a standard curve of the trace and trace benzyl ammonium chloride collector is established, namely a trace and trace benzyl ammonium chloride collector standard solution is prepared, an ultraviolet visible spectrophotometer is adopted, ultrapure water is used as a background, and spectrum scanning is carried out on the trace and trace benzyl ammonium chloride collector standard solution in a wavelength range of 185-800 nm; selecting proper absorption wavelength as ultraviolet detection wavelength of trace and trace benzyl ammonium chloride collecting agent, fixing different detection wavelengths to respectively perform photometry of trace and trace solutions, establishing relationship between concentration and absorbance of the trace and trace benzyl ammonium chloride solution, and drawing a standard curve; The concentration of the trace benzyl ammonium chloride collector standard solution is 5-100ppm, the concentration of the trace benzyl ammonium chloride collector standard solution is 0.1-5ppm, the ultraviolet detection wavelength of the trace benzyl ammonium chloride collector is 200-220nm, and the ultraviolet detection wavelength of the trace benzyl ammonium chloride collector is 185-200nm; Respectively carrying out photometry on the background solution detected by ultraviolet and the sample to be detected by adopting an ultraviolet-visible spectrophotometer, and determining the content of the benzyl ammonium chloride collector in the sample to be detected according to the standard curve of the established trace and trace benzyl ammonium chloride collectors; Calculating the adsorption quantity of the benzyl ammonium chloride collector on the mineral surface through the difference value of the initial concentration of the benzyl ammonium chloride collector and the residual concentration in the sample to be detected, wherein the calculation formula is as follows: ; Wherein Γ is adsorption capacity, kg/m 2 ;c m0 and c m1 are initial concentration and residual concentration of benzyl ammonium chloride collector, g/mL respectively, V is volume of solution, mL, m is mass of mineral sample, g, S is specific surface area of pure mineral, and m 2 /Kg.

Description

Quantitative test method for adsorption capacity of benzyl ammonium chloride collector on mineral surface in flotation process Technical Field The invention relates to the technical field of collophanite flotation, in particular to a method for detecting adsorption quantity of a benzyl ammonium chloride collector on the surface of a mineral, and particularly relates to a quantitative test method for adsorption quantity of the benzyl ammonium chloride collector on the surface of the mineral in a flotation process. Background 70% Of phosphorite resources in China belong to sedimentary rock type phosphorite, and the useful mineral apatite in the phosphorus-rich sedimentary ore deposit is often associated with gangue minerals such as potassium feldspar, dolomite and the like, the average grade of P 2O5 is low, the collophanite is the main material, the ore embedding granularity is fine, and the sorting difficulty is high. The collophanite flotation technology is a process for realizing concentrate enrichment through froth flotation by utilizing the adsorption difference between different ores and collectors, and is an important way for realizing phosphorite recovery. Benzyl ammonium chloride collectors are of great interest as important collectors for reverse flotation of collophanite. The flotation effect is directly related to the adsorption quantity of the collector on the mineral surface, excessive collector consumption can cause a series of problems such as medicament waste, abnormal fluctuation of mineral separation indexes, poor precision selectivity, phosphorus loss and the like, and the too small collector consumption can cause phosphorus loss. Therefore, in order to effectively regulate and control the dosage of the collector, the operation of a black box is avoided, and the accurate analysis of the adsorption quantity on the surface of the mineral is particularly critical. Wang Dianzuo et al discloses "application of absorption spectroscopy in flotation research" that the amount of absorption of ultraviolet light in a flotation process is measured by bringing a reagent solution into contact with a mineral, measuring the concentration of an equilibrium solution, calculating the amount of absorption from the difference between the equilibrium solution and the initial concentration, desorbing the adsorbed reagent by treating the reacted mineral with an appropriate solvent, and measuring the concentration thereof to calculate the amount of absorption. CN113834890B discloses a method for accurately and quantitatively analyzing the adsorption quantity of a mineral surface sodium oleate collector in a flotation process, which comprises the following steps of (1) adding sodium oleate into ore pulp, oscillating, centrifuging after adsorption reaches equilibrium, taking supernatant as a liquid to be tested, (2) adding excessive concentrated H2SO4 into the liquid to be tested to convert sodium oleate into oleic acid, then carrying out extraction separation to obtain an oil phase containing oleic acid, (3) carrying out methyl esterification treatment on the oleic acid to obtain methyl oleate, and (4) carrying out detection analysis on a methyl oleate organic phase containing an internal standard of methyl heptadecanoate by a gas chromatography-mass spectrometer, and then calculating the adsorption quantity of the mineral surface sodium oleate according to detection analysis results. As previously mentioned, common methods for measuring adsorption include extraction, high performance liquid chromatography, infrared spectroscopy, ion chromatography, etc., which use toxic agents such as benzene, have peaks that show no significant excesses from the measurement range due to too low a trace collector concentration, and the water environment in the flotation process contains various anions and cations (such as Ca 2+/Mg2+/F-/Cl-/K-/PO43-/SO42-, etc.), other ion interferences that make it impossible to define adsorption of benzyl ammonium chloride collectors by measuring chlorine content. In addition, the benzyl ammonium chloride collector has both hydrophilic end and hydrophobic end, so that the measurement accuracy cannot be influenced by complete extraction, the extraction process is complex in operation, additional solvent is required to be introduced, environmental pollution is caused, the measurement cost is increased, the adsorption degree of ores is different at different moments in the flotation process, the concentration of the benzyl ammonium chloride collector remained in a water body spans a large range, and the measurement accuracy is directly influenced by dilution or concentration, so that the development of a method for accurately measuring the adsorption quantity of the benzyl ammonium chloride collector in the flotation process is needed. Disclosure of Invention In order to solve the problems, the invention provides a quantitative test method for the adsorption quantity of a benzyl ammonium chloride c