CN113030067B - Method for rapidly identifying rare earth grade of weathering crust elution-deposited rare earth ore in field - Google Patents
Method for rapidly identifying rare earth grade of weathering crust elution-deposited rare earth ore in field Download PDFInfo
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Abstract
The invention provides a field rapid identification method for rare earth grade of weathering crust eluviation type rare earth ore, which comprises the following steps: (1) sampling: weighing a weathering crust elution type rare earth ore sample to be measured, and recording the mass of the weighed sample to be measured as m; (2) preparing an extract: leaching the sample to be measured weighed in the step (1) by using an ammonium sulfate solution to prepare a leaching solution, wherein the volume of the ammonium sulfate solution is marked as V; (3) and (3) measuring turbidity: slowly dripping the leaching solution prepared in the step (2) into a turbidity bottle containing a dispersing agent and an oxalic acid solution, immediately mixing uniformly after dripping, and measuring the turbidity T of the system by using a turbidimeter; (4) calculating the grade of the rare earth: and (3) calculating the grade of the rare earth in the rare earth ore according to the formula (2). The invention establishes the conversion relation between the turbidity of the rare earth oxalate suspension and the rare earth concentration, and the field reconnaissance only needs to measure the turbidity to identify the rare earth grade, which is simpler, more convenient and faster than the direct measurement of the rare earth concentration.
Description
Technical Field
The invention belongs to the field of chemical analysis, and particularly relates to a weathering crust elution-deposited rare earth ore rare earth grade field rapid identification method.
Background
The weathering crust eluviation type rare earth ore is a unique valuable resource rich in medium-heavy rare earth in south China, which accounts for about 2.6 percent of the total rare earth resource in China, but provides more than 95 percent of the heavy rare earth in the world. The demand of the modern industry on rare earth is continuously increased, and the investigation and the search of new weathering crust elution accumulation type rare earth ore resources have important significance for relieving the current nervous supply situation.
At present, an inductively coupled plasma spectrometer/mass spectrometer (ICP-OES, ICP-MS) is often adopted as an accurate determination method for the content of rare earth, but the method needs a large-scale and expensive measuring instrument, and cannot be used for field investigation. The improved EDTA titration method based on national standard GB/T14635-2008 of Buruan et al is used for rapidly determining the rare earth content in the field (CN 102297862A). However, the method has the problems of insensitive color change, complex and portable required reagents, complex operation process and the like (ascorbic acid, sulfosalicylic acid, hexamethylenetetramine, xylenol orange and EDTA standard solution are required to be added in the leaching solution in sequence). The crown Hongli proposes that saturated oxalic acid solution is adopted to precipitate the ammonium sulfate leaching solution of the drilling sample, and the rare earth grade is judged by a method of observing the morphology of the precipitated product by naked eyes (CN 106353316A). The method is simple and convenient for field operation, but the accuracy of judging the rare earth content by observing the state of the precipitate by naked eyes is low. For example, the method indicates that when the soaking solution is light white, dark white, white precipitate and white precipitate are snowy, the rare earth grade belongs to different intervals. However, in the actual operation process, the states of the precipitates are difficult to distinguish by naked eyes, and the content of the rare earth cannot be accurately judged. Meanwhile, the particle size of the rare earth oxalate is influenced by factors such as feeding mode, stirring intensity, temperature, concentration, acidity and the like when the rare earth oxalate is precipitated, and the form of the precipitate is not completely caused by the concentration of the rare earth. In addition, particles can aggregate with time when oxalate precipitates, and misjudgment is easily caused when samples are observed at different times.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide a field rapid identification method for rare earth grade of weathering crust elution-deposited rare earth ore, which can rapidly and accurately determine the rare earth grade of weathering crust elution-deposited rare earth ore in the field, and is convenient and efficient.
In order to achieve the purpose, the invention adopts the following technical scheme:
a weathering crust eluviation type rare earth ore rare earth grade field rapid identification method comprises the following steps:
(1) sampling: weighing a weathering crust elution type rare earth ore sample to be measured, and recording the mass of the weighed sample to be measured as m;
(2) preparing an extract: leaching the sample to be measured weighed in the step (1) with an ammonium sulfate solution to prepare a leaching solution, wherein the volume of the ammonium sulfate solution is recorded as V;
(3) and (3) measuring turbidity: slowly dripping the leaching solution prepared in the step (2) into a turbidity bottle containing an oxalic acid solution and a dispersing agent, immediately mixing uniformly after dripping, and measuring the turbidity T of the system by using a turbidimeter;
(4) calculating the grade of the rare earth:
the concentration of the rare earth solution is calculated according to the formula (1),
the rare earth concentration calculation formula of the leaching solution is as follows:
C＝1.5912T+120.6926 R 2 ＝0.9939 (1)
calculating the grade of the rare earth in the rare earth ore according to the formula (2),
the rare earth grade calculation formula is as follows:
in the formula: REO-rare earth grade, mg/kg;
c, leaching solution rare earth concentration, unit mg/L;
t-turbidity, in NTU;
v is the volume dosage of ammonium sulfate, and the unit is mL;
m is the mass of the sample to be measured, unit g;
C w -water content of the sample to be tested, in%; measuring the moisture of a sample to be measured by adopting a rapid moisture tester;
R 2 -linear correlation coefficient.
Further, in the step (1), the mass of the sample to be detected is 50-200 g.
Further, the mass fraction of the ammonium sulfate solution in the step (2) is 2-5%.
Further, the volume of the ammonium sulfate solution in the step (2) is 50-200 mL.
Further, the leaching solution in the step (2) is prepared by the following steps: folding the filter paper into a funnel shape, and placing the filter paper in the funnel; placing the funnel on the conical flask; pouring the sample to be measured weighed in the step (1) into a transparent plastic bottle, weighing 50-200mL of ammonium sulfate solution to immerse the sample to be measured in the plastic bottle, recording the volume of the ammonium sulfate solution as V, and shaking the sample to be measured and the ammonium sulfate leaching solution for 1-2min to be uniform; the well-mixed sample was poured into a funnel and the leachate was dropped into the flask through the funnel mouth.
Further, the concentration of the oxalic acid solution in the step (3) is 0.2 g/L.
Further, in the step (3), the dispersing agent is selected from one or more of sodium hexametaphosphate, sodium pyrophosphate and ethanol.
Further, the mass fraction of the dispersant in the step (3) is 0.1-1%.
Further, the turbidity measuring process of step (3) is as follows: transferring the oxalic acid solution and injecting into a turbidity bottle; dripping a dispersing agent into the oxalic acid solution; then, the leaching solution in the step (2) is slowly dripped into the turbidity bottle, and the solution is slowly oscillated in the dripping process to prevent the precipitate from agglomerating; shaking up immediately after the dropwise addition is finished, and measuring the turbidity T of the system by using a turbidimeter.
Further, the turbidity measuring process of step (3) is as follows: using a liquid transfer gun to transfer 15mL of oxalic acid solution into a 20mL turbidity bottle; dripping 2 drops of dispersing agent into the oxalic acid solution by adopting a rubber head dropper; then, using a syringe injector to transfer 5mL of the leaching solution obtained in the step (2) to be slowly dropped into the turbidity bottle, and slowly oscillating in the dropping process to prevent precipitates from agglomerating; shaking up immediately after the dropwise addition is finished, and measuring the turbidity T of the system by using a turbidimeter.
Further, the formula (1) and the formula (2) in the step (4) are obtained according to the following method: (1) sampling: weighing a plurality of samples to be detected, wherein the specific mass of the samples to be detected is recorded as m; (2) preparing an extract: pouring the sample to be detected weighed in the step (1) into a container, immersing the sample to be detected in the container by using ammonium sulfate solution, recording the volume of the ammonium sulfate solution as V, shaking the sample to be detected and the ammonium sulfate leaching solution for 1-2min till the samples are uniform, and filtering the fully mixed sample to obtain the leaching solution; (3) and (3) measuring turbidity: transferring the oxalic acid solution and injecting into a turbidity bottle; dripping a dispersing agent into the oxalic acid solution; then, the leaching solution in the step (2) is slowly dripped into the turbidity bottle, and the solution is slowly oscillated in the dripping process to prevent the precipitate from agglomerating; shaking up immediately after the dropwise adding is finished, and measuring the turbidity, T, of the system by using a turbidimeter; (4) and (3) concentration measurement: measuring the concentration of 17 rare earth elements in the leaching solution in the step (2) by adopting an inductively coupled plasma spectrometer (ICP-OES), and accumulating to obtain the total rare earth concentration; (5) fitting: establishing a turbidity-concentration relation scatter diagram by taking the turbidity measured in the step (3) as an abscissa and the concentration measured in the step (4) as an ordinate, and performing linear fitting on the scatter diagram to obtain a formula (1); (6) correcting the formula: and (3) measuring the moisture of the sample to be measured, and performing quality correction on the formula (1) to obtain a formula (2).
Further, the formula (1) and the formula (2) in the step (4) are obtained according to the following method: (1) weighing: weighing a plurality of samples to be detected with the mass of 50-200g by adopting a portable electronic scale, wherein the specific mass of the samples to be detected is recorded as m; (2) leaching: folding the filter paper into a funnel shape, and placing the filter paper in the funnel; placing the funnel on the conical flask; pouring the sample to be measured weighed in the step (1) into a transparent plastic bottle, measuring 50-200mL of ammonium sulfate solution to immerse the sample to be measured in the plastic bottle, wherein the volume of the ammonium sulfate solution is marked as V, fully shaking the sample to be measured and ammonium sulfate leaching solution for 1-2min, pouring the fully mixed sample into a funnel, and dripping the leaching solution into a conical bottle from the mouth of the funnel; (3) and (3) measuring turbidity: using a liquid transfer gun to transfer 15mL of oxalic acid solution into a 20mL turbidity bottle; dripping 2 drops of dispersing agent into the oxalic acid solution by using a rubber head dropper; then, using a syringe injector to transfer 5mL of the leaching solution obtained in the step (2) to be slowly dropped into the turbidity bottle, and slowly oscillating in the dropping process to prevent precipitates from agglomerating; shaking up immediately after the dropwise adding is finished, and measuring the turbidity, T, of the system by using a turbidimeter; (4) and (3) concentration measurement: measuring the concentrations of the 17 rare earth elements in the leaching solution in the step (2) by adopting an inductively coupled plasma spectrometer (ICP-OES), and accumulating to obtain the total rare earth concentration; (5) fitting: establishing a turbidity-concentration relation scatter diagram by taking the turbidity measured in the step (3) as an abscissa and the concentration measured in the step (4) as an ordinate, and performing linear fitting on the scatter diagram to obtain a formula (1); (6) correcting the formula: measuring the moisture of a sample to be measured, and performing quality correction on the formula (1) to obtain a formula (2); in the formula: REO-rare earth grade, mg/kg; c, leaching liquid rare earth concentration, unit mg/L; t-turbidity, monoBit NTU; v is the volume dosage of ammonium sulfate, unit mL; m is the mass of the sample to be measured, unit g; c w -water content of the sample to be tested, in%; measuring the moisture of a sample to be measured by adopting a rapid moisture tester; r 2 -linear correlation coefficient.
Further, the detection tool used in the method comprises: ammonium sulfate solution, oxalic acid solution, portable turbidimeter, portable electronic scale, pipette, 20mL turbidimeter bottle, filter paper, glass funnel, conical flask and graduated cylinder, syringe injector, rubber dropper, transparent plastic bottle, and rapid moisture meter.
The principle of the method of the invention lies in that:
the principle of converting the rare earth concentration by turbidity is utilized: the inventor finds out in the research that: when saturated oxalic acid solution is slowly dripped into the leaching solution of the rare earth ammonium sulfate ore, rare earth, iron, aluminum and other metal impurities in the leaching solution can generate oxalate precipitation, so that the leaching solution becomes turbid, and the turbidity of the system suspension liquid and the concentration of the rare earth present certain correlation. However, the particle size of the oxalate precipitate is affected by factors such as the feeding mode, the stirring intensity, the temperature, the concentration, the acidity, the precipitation time and the like, so that the turbidity value of the oxalate precipitate is unstable. A method for stabilizing the turbidity value of oxalate is obtained through experiments, and the concentration of ammonium sulfate, the concentration of oxalic acid, the type of a dispersing agent, the concentration of the dispersing agent, the using amount of the dispersing agent and a feeding mode are determined. The method is adopted to analyze the instantaneous turbidity and the rare earth concentration of oxalate of 500 rare earth ore ammonium sulfate leachate samples, and the relationship between the turbidity and the rare earth concentration is established by depending on big data, compared with the prior art in which the state of a precipitate is observed by naked eyes, the accuracy is obviously improved, the rare earth grade can be accurate to 3 bits after a decimal point, and the measurement error is within 10 percent.
And (3) quality correction: the formula corrects the quality of a weighed sample on the basis of a large amount of field rare earth ore moisture data, and a rapid moisture tester is adopted to measure the moisture of the sample to be measured.
Compared with the prior art, the invention has the following beneficial effects:
1. the reagent and the method for stabilizing the turbidity value of the oxalate suspension are discovered, the conversion relation between the turbidity of the rare earth oxalate suspension and the rare earth concentration is established based on the big data experiment result, the grade of the rare earth can be identified only by measuring the turbidity in the field, and the method is simpler, more convenient and faster than the method for directly measuring the rare earth concentration;
2. the conversion formula is established based on the oxalate suspension turbidity-rare earth concentration of the natural rare earth ore sample ammonium sulfate leaching solution, is not a rare earth standard solution prepared manually, and already contains influences possibly generated by oxalate precipitation, rare earth distribution and solution pH of impurity metals, the grade of the obtained rare earth is more accurate, and the grade of the rare earth can reach 3 bits after a decimal point through verification, and the measurement error is within 10%.
Drawings
FIG. 1 is a linear fit of turbidity versus rare earth concentration for an oxalate suspension according to the invention.
Detailed Description
In order to enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be further described in detail with reference to the following examples.
Examples 1 to 30
(1) Weighing: weighing 50-200g of a sample to be measured by adopting a portable electronic scale, and recording the specific mass as m; (2) leaching: folding the filter paper into a funnel shape, and placing the filter paper in the funnel; placing the funnel on the conical flask; pouring the sample to be measured weighed in the step (1) into a transparent plastic bottle, weighing 50-200mL of ammonium sulfate solution to immerse the sample to be measured in the plastic bottle, recording the volume of the saturated ammonium sulfate solution as V, and shaking the sample to be measured and the ammonium sulfate leaching solution for 2min to be uniform; the well-mixed sample was poured into a funnel and the leachate was dropped into the flask through the funnel mouth. (3) And (3) measuring turbidity: using a liquid transfer gun to transfer 15mL of oxalic acid solution (0.2g/L) into a 20mL turbidity bottle; then 2 drops of dispersant solution (sodium hexametaphosphate solution with the mass fraction of 0.1 percent) is added; and (3) transferring 5mL of the leaching solution prepared in the step (2) by using a syringe injector, slowly dripping the leaching solution into the turbidity bottle, shaking up immediately after dripping, and measuring the turbidity and T of the system by using a turbidimeter (Shanghai Yuefeng, SGZ-1000 BS). (4) And (3) concentration measurement: measuring the concentrations of the 17 rare earth elements in the leaching solution in the step (2) by adopting an inductively coupled plasma spectrometer (ICP-OES) (Agilent, ICPOES730 in the USA), and accumulating to obtain the total rare earth concentration; (5) fitting: establishing a turbidity-concentration relation scatter diagram by taking the turbidity measured in the step (3) as an abscissa and the concentration measured in the step (4) as an ordinate, and performing linear fitting on the scatter diagram to obtain a formula (1) as shown in fig. 1; (6) correcting the formula: the field weathering crust leaching type rare earth ore usually contains 30-40% of water, a rapid moisture tester is adopted to measure the water content of a sample to be measured, and the formula (1) is subjected to quality correction to obtain the formula (2). (7) And (3) obtaining the calculated concentration of the sample to be detected by using a formula (1), and calculating the rare earth grade of the weathering crust elution-deposited rare earth ore in the field by using a formula (2). The measurement specific data and calculation data for each example are shown in table 1. FIG. 1 is a graph showing a linear fit of turbidity to rare earth concentration for an oxalate suspension according to the invention. As can be seen from Table 1, the rare earth grade calculated by the formula (2) and the measured rare earth grade in each example can be well matched.
The rare earth concentration calculation formula of the leaching solution is as follows:
C＝1.5912T+120.6926 R 2 ＝0.9939 (1)
the rare earth grade calculation formula is as follows:
in the formula: REO-rare earth grade, mg/kg;
c, leaching solution rare earth concentration, unit mg/L;
t-turbidity, in NTU;
v is the volume dosage of ammonium sulfate, unit mL;
m is the mass of the sample to be measured, unit g;
C w -water content of the sample to be tested, in%; measuring the moisture of a sample to be measured by adopting a rapid moisture tester;
R 2 -linear correlation coefficient.
TABLE 1 results of examples 1-30
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention. Those skilled in the art can make various changes, modifications and equivalent arrangements, which are equivalent to the embodiments of the present invention, without departing from the spirit and scope of the present invention, and which may be made by utilizing the techniques disclosed above; meanwhile, any changes, modifications and variations of the above-described embodiments, which are equivalent to those of the technical spirit of the present invention, are within the scope of the technical solution of the present invention.
Claims (6)
1. A weathering crust eluviation type rare earth ore rare earth grade field rapid identification method is characterized by comprising the following steps:
(1) sampling: weighing a weathering crust elution type rare earth ore sample to be measured, and recording the mass of the weighed sample to be measured as m;
(2) preparing an extract: leaching the sample to be measured weighed in the step (1) by using an ammonium sulfate solution to prepare a leaching solution, wherein the volume of the ammonium sulfate solution is marked as V;
(3) and (3) measuring turbidity: slowly dripping the leaching solution prepared in the step (2) into a turbidity bottle containing an oxalic acid solution and a dispersing agent, immediately mixing uniformly after dripping, and measuring the turbidity T of the system by using a turbidimeter; the turbidity measurement procedure was as follows: transferring the oxalic acid solution and injecting into a turbidity bottle; dripping a dispersing agent into the oxalic acid solution; then, the leaching solution in the step (2) is slowly dripped into the turbidity bottle, and the solution is slowly oscillated in the dripping process to prevent the precipitate from agglomerating; shaking up immediately after the dropwise adding is finished, and measuring the turbidity T of the system by using a turbidimeter; the concentration of the oxalic acid solution is 0.2 g/L; the dispersing agent is selected from one or more of sodium hexametaphosphate and sodium pyrophosphate; the mass fraction of the dispersant is 0.1-1%;
(4) calculating the grade of the rare earth:
calculating the rare earth concentration of the leaching solution according to the formula (1),
the rare earth concentration calculation formula of the leaching solution is as follows:
C＝1.5912T+120.6926 R 2 ＝0.9939 (1)
calculating the grade of the rare earth in the rare earth ore according to the formula (2),
the rare earth grade calculation formula is as follows:
in the formula: REO-rare earth grade, mg/kg;
c, leaching liquid rare earth concentration, unit mg/L;
t-turbidity, in NTU;
v is the volume dosage of ammonium sulfate, unit mL;
m is the mass of the sample to be measured in unit g;
C w -water content of the sample to be tested, in%;
R 2 -linear correlation coefficient.
2. The method according to claim 1, wherein in step (1), the mass of the sample to be tested is 50-200 g.
3. The method of claim 1, wherein the mass fraction of the ammonium sulfate solution in step (2) is 2% -5%.
4. The method of claim 1, wherein the volume of the ammonium sulfate solution in step (2) is 50-200 mL.
5. The method according to claim 1, wherein the leachate in step (2) is prepared as follows: folding the filter paper into a funnel shape, and placing the filter paper in the funnel; placing the funnel on the conical flask; pouring the sample to be measured weighed in the step (1) into a transparent plastic bottle, weighing 50-200mL of ammonium sulfate solution to immerse the sample to be measured in the plastic bottle, recording the volume of the ammonium sulfate solution as V, and shaking the sample to be measured and the ammonium sulfate leaching solution for 1-2min to be uniform; the well-mixed sample was poured into a funnel and the leachate was dropped into the flask through the funnel mouth.
6. The method according to claim 1, wherein the formula (1) and the formula (2) in the step (4) are obtained as follows: (1) sampling: weighing a plurality of samples to be detected, wherein the specific mass of the samples to be detected is recorded as m; (2) preparing an extract: pouring the sample to be detected weighed in the step (1) into a container, immersing the sample to be detected in the container by using ammonium sulfate solution, recording the volume of the ammonium sulfate solution as V, shaking the sample to be detected and the ammonium sulfate solution for 1-2min till the samples are uniform, and filtering the fully mixed sample to obtain an extract; (3) and (3) measuring turbidity: transferring the oxalic acid solution and injecting into a turbidity bottle; dripping a dispersing agent into the oxalic acid solution; then, the leaching solution in the step (2) is slowly dripped into the turbidity bottle, and the solution is slowly oscillated in the dripping process to prevent the precipitate from agglomerating; shaking up immediately after the dropwise adding is finished, and measuring the turbidity, T, of the system by using a turbidimeter; (4) and (3) concentration measurement: measuring the concentration of 17 rare earth elements in the leaching solution in the step (2) by using an inductively coupled plasma spectrometer, and accumulating to obtain the total rare earth concentration; (5) fitting: establishing a turbidity-concentration relation scatter diagram by taking the turbidity measured in the step (3) as a horizontal coordinate and the concentration measured in the step (4) as a vertical coordinate, and performing linear fitting on the scatter diagram to obtain a formula (1); (6) correcting the formula: and (3) measuring the moisture of the sample to be measured, and performing quality correction on the formula (1) to obtain a formula (2).
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| CN102297862A (en) * | 2011-07-20 | 2011-12-28 | 武汉工程大学 | Method for rapidly measuring rare earth grade of ion absorpt deposit in field |
| CN103184356B (en) * | 2011-12-28 | 2014-12-17 | 有研稀土新材料股份有限公司 | Treatment method for rare earth phosphate rock and enrichment method for rare earth |
| CN205719995U (en) * | 2016-05-12 | 2016-11-23 | 江西理工大学 | A kind of detection device for quickly measuring ion adsorption type re content |
| CN106353316A (en) * | 2016-09-09 | 2017-01-25 | 江西稀有金属钨业控股集团有限公司 | Quick testing method for outdoor exploration of ionic rare earth |
| CN106702181B (en) * | 2016-11-14 | 2019-04-16 | 江西理工大学 | A kind of leaching method improving ion adsorption type rare earth ore leaching rate |
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