CN111537328A - Pretreatment method for chromium ore by microwave digestion acid melting method and chromium production method - Google Patents
Pretreatment method for chromium ore by microwave digestion acid melting method and chromium production method Download PDFInfo
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Abstract
The invention belongs to the technical field of ferrochrome alloy production, and discloses a pretreatment method for putting a chromite sample into a microwave digestion acid-melting method and a chromium production method, wherein the pretreatment technology of an ultrahigh pressure microwave digestion acid-melting method is adopted for the chromite sample, a certain amount of chromite sample is weighed and placed in a polytetrafluoroethylene digestion tank, a certain amount of water is added to uniformly mix the sample, a certain amount of sulfuric acid, phosphoric acid and fluoboric acid are added, and the chromium alloy is covered and sleeved; placing the mixture in a turntable, placing the mixture in a microwave digestion instrument, setting parameters of an ultrahigh pressure instrument, and starting up the microwave digestion instrument; after digestion, the sample is cooled to room temperature, and then the sample liquid is transferred to a bottle to be tested. The optimized experiment of the instrument parameters and the pretreatment conditions uses the national standard substance number GSBD33001.2-94 chromite for comparison, and the marked values are as follows: cr (chromium) component2O3：38.80％；Fe：17.58％。
Description
Technical Field
The invention belongs to the technical field of ferrochrome alloy production, and particularly relates to a pretreatment method for a chromium ore by a microwave digestion acid melting method and a chromium production method.
Background
At present, chromium is widely used in metallurgical industry, refractory material and chemical industry as an important strategic resource. The chromium iron alloy is mainly used as an important raw material for producing stainless steel in the metallurgical industry in the form of chromium iron alloy, is mainly used for producing chromium iron alloy and metal chromium, can greatly enhance the hardness and corrosion resistance of the stainless steel, is mainly used for smelting special alloy with elements such as cobalt, nickel, tungsten and the like, and is an indispensable material for aviation, aerospace, automobiles, shipbuilding, gun guns, missiles, rockets, naval vessels and the like in the national defense industry. Chromite is mainly used in chemical industry for producing sodium dichromate and further for preparing other chromium compounds, and is used in industries of pigment, textile, electroplating, leather making and the like, and can also be used for preparing catalysts, catalysts and the like. Chromite is a shortage mineral species in China, has small reserves and low yield, more than 80 percent of annual consumption amount depends on import, and along with the increase of import amount, the chromite brings vitality for the development of national economy of China and also possibly brings toxic and harmful elements to pollute soil, water and atmosphere and influence human health. The national environmental protection is increasingly important, and the monitoring of imported chromite is urgent, so that the control of harmful elements in the chromite ore becomes one of the main measures for improving the environmental quality. Therefore, it is necessary to detect various elements including harmful elements in the chromite ore and to study methods thereof.
The chromite belongs to one of refractory ore species, the prior chromite pretreatment technology comprises an alkali fusion method and an acid fusion method, the alkali fusion method is complex and tedious to operate and has long time, the salt content in sample liquid after the pretreatment is finished is high, the requirement on instruments is high, the measurement sensitivity is not strong, and the measurement result is not accurate enough. However, the common acid melting method cannot completely dissolve the chromium ore, the microwave digestion technology is more and more applied to the pretreatment of the chromite sample in recent years, but the common high-pressure microwave digestion technology cannot completely dissolve various chromites, and the microwave digestion of the chromite sample under the ultrahigh pressure condition has been studied, but the existing problems cannot be completely solved, because the chromite sample is a refractory sample, and any acid can not be dissolved almost under the common condition, the inspection period is prolonged, and the operation is complicated.
Through the above analysis, the problems and defects of the prior art are as follows:
(1) the prior chromite pretreatment technology has the disadvantages of complex and tedious operation and long time, and the sample liquid after pretreatment has high salinity, high requirement on instruments, low measurement sensitivity and inaccurate measurement result.
(2) The common acid melting method can not completely dissolve the chromium ore; the common high-pressure microwave digestion technology can not completely dissolve various chromite, and the microwave digestion of the chromite sample under the ultrahigh-pressure condition has been studied, but can not completely solve the existing problems.
The difficulty in solving the above problems and defects is: the acid melting method without the ultrahigh pressure microwave digestion technology cannot completely dissolve chromium ore, black slag occurs, an accurate analysis result cannot be obtained, the pretreatment time of the alkali melting method is long, high-concentration salt can be brought, the detection limit and stability of an instrument are influenced during measurement, the sample weighing amount, the selection of digestion acid, the consumption of digestion acid, the selection of digestion power and digestion time need to be considered under the ultrahigh pressure condition, and the problem of precipitation white slag needs to be solved.
The significance of solving the problems and the defects is as follows: the method has the advantages of simplicity, convenience, rapidness, accuracy, reliability and the like, well solves the problems of high blank value, large amount of matrix salts, long sample melting time and the like in chromium ore dissolution, can be used for detecting large batches of chromium ore in a laboratory, greatly improves the working efficiency and the analysis accuracy of laboratory personnel, can further increase and accelerate the monitoring of harmful elements in imported chromite, and plays a positive role in protecting the natural environment of China and promoting the trade of chromite.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a pretreatment method for a chromium ore microwave digestion acid melting method and a chromium production method.
The invention is realized in such a way that a pretreatment method for putting a chromium ore microwave digestion acid melting method into a pretreatment device is characterized in that the pretreatment method for putting the chromium ore microwave digestion acid melting method into the pretreatment device comprises the following steps:
firstly, weighing 0.2g of chromite ore sample, and placing the chromite ore sample in a polytetrafluoroethylene digestion tank;
secondly, adding 1.0ml of water to uniformly mix the samples, adding 8ml of sulfuric acid, 5ml of phosphoric acid and 1ml of fluoboric acid, and covering and sleeving; placing in a turntable, placing in a microwave digestion instrument, and setting parameters of the ultrahigh pressure instrument (the output power of the microwave digestion instrument is 1200W, the temperature rise program is that the time required for rising from normal temperature to 250 ℃ under the condition of keeping 1200W power is 30min, and the time for keeping at 250 ℃ is 40 min); starting up the machine to carry out microwave digestion;
and thirdly, after the digestion is finished, transferring the sample liquid into a bottle to be tested after the sample is cooled to room temperature.
Further, the microwave digestion acid melting method of the chromium ore is put into the ultrahigh pressure condition of the pretreatment method: the output power of the microwave digestion instrument is 800W-1200W, and the temperature rising program is as follows: the time required for raising the temperature from the normal temperature to 220-250 ℃ under the condition of keeping constant power is 20-35min, and the time for reaching the temperature is 25-40 min.
Further, the selection and quantification of the reagent of the pretreatment method in the chromium ore microwave digestion acid melting method are as follows: 6mL to 8mL of sulfuric acid, 4mL to 5.5mL of phosphoric acid and 0.5mL to 1.5mL of fluoroboric acid.
Further, the sample weight of the chromium ore put into the pretreatment method by the microwave digestion acid melting method is 0.10g-0.25 g.
Further, the chromium ore microwave digestion acid melting method is placed into a digestion tank for weighing the sample of the pretreatment method, then the sample is wetted by quantitative deionized water of 0.5ml to 2.5ml, the sample water drops of the chromium ore are uniformly mixed, and then acid is added.
Another object of the present invention is to provide a process for producing ferrochrome alloy using the said chromium ore microwave digestion acid melting method into pretreatment method.
The invention also aims to provide a method for producing metallic chromium by using the chromium ore microwave digestion acid melting method and putting the method into a pretreatment method.
TABLE 1 analysis results of the original and conventional methods for the measured value of chromite imported from various countries
As can be seen from the analysis results in Table 1, the measured values of the chromite imported from various countries by using the method are consistent with the measured values of the traditional method, and the effectiveness of the scheme is further illustrated.
By combining all the technical schemes, the invention has the advantages and positive effects that: the invention adopts a pretreatment technology of an ultrahigh pressure microwave digestion acid melting method for a chromite sample, and the process comprises the following steps: weighing a certain amount of chromite ore sample, placing the chromite ore sample in a polytetrafluoroethylene digestion tank, adding a certain amount of water to uniformly mix the sample, adding a certain amount of sulfuric acid, phosphoric acid and fluoboric acid, and covering and sleeving. Placing the mixture in a turntable, placing the mixture into a microwave digestion instrument, setting parameters of an ultrahigh pressure instrument, and starting the microwave digestion instrument to carry out microwave digestion. After digestion, the sample is cooled to room temperature, and then the sample liquid is transferred to a bottle to be tested. The optimized experiment of the instrument parameters and the pretreatment conditions uses the national standard substance number GSBD33001.2-94 chromite for comparison, and the marked values are as follows: cr (chromium) component2O3：38.80％；Fe：17.58％。
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FIG. 1 is a flow chart of a pretreatment method for microwave digestion of acid melting of chromium ore according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a pretreatment method for a chromium ore by a microwave digestion acid melting method and a chromium production method, and the invention is described in detail with reference to the attached drawings.
As shown in fig. 1, the method for pretreating chromium ore by microwave digestion and acid melting provided by the embodiment of the present invention includes the following steps:
s101: weighing a certain amount of chromite stone sample, and placing the chromite stone sample in a polytetrafluoroethylene digestion tank;
s102: adding a certain amount of water to uniformly mix the sample, adding a certain amount of sulfuric acid, phosphoric acid and fluoroboric acid, and covering and sleeving; placing the mixture in a turntable, placing the mixture in a microwave digestion instrument, setting parameters of an ultrahigh pressure instrument, and starting up the microwave digestion instrument;
s103: after digestion, the sample is cooled to room temperature, and then the sample liquid is transferred to a bottle to be tested.
The technical effects of the present invention will be described in detail with reference to experiments.
The technical conditions of the pretreatment of the invention comprise:
(1) ultrahigh pressure conditions: the instrument is a Meilstone microwave digestion instrument (ETHOSONE), the output power of the microwave digestion instrument is 800W-1200W, and the temperature rising program comprises the following steps: the time required for raising the temperature from the normal temperature to 220-250 ℃ under the condition of keeping constant power is 20-35min, and the time for reaching the temperature is 25-40 min; according to the judgment of the experimental result, the temperature rise program and the output power are selected to be most effective in completely dissolving the chromite sample.
TABLE 2 microwave digestion procedure sample dissolution Experimental results for different procedures
2. Selection and quantification of reagents: 6mL to 8mL of sulfuric acid, 4mL to 5.5mL of phosphoric acid and 0.5mL to 1.5mL of fluoroboric acid, wherein the phosphoric acid plays a very strong dissolving role for difficultly soluble ore species, but the boiling point of the phosphoric acid is lower than that of the sulfuric acid, but the phosphoric acid is easy to dehydrate to separate out white precipitates, so the phosphoric acid cannot play a dissolving role when the amount of the phosphoric acid is too small, and the sample dissolving temperature is reduced when the amount of the phosphoric acid is too large, so a proper amount of phosphoric acid needs to be comprehensively considered, and the fluoroboric acid is selected to replace hydrofluoric acid because the two can achieve the aim of dissolving silicon by considering the same way, and the excessive fluoroboric acid has little damage to glassware.
TABLE 3 results of different sample-dissolving acids and different amounts
3. Selection of sample size: when the sample mass is too small, the sample can be completely digested under the same digestion condition, but the sample is not representative and the system error is increased, when the sample mass is too large, undissolved black residues appear after dissolution under the same digestion condition, which indicates that the black residues are undissolved chromite samples, so the result of the dissolved sample liquid measured by an on-machine method or a chemical method is not accurate enough, and the sample weighing amount is selected to be 0.10g-0.25g in the experiment considering that the weighed sample must be representative and universal and consistent with industrial standards and national standards.
Table 4 results of different sample weights
4. Weighing the sample into a digestion tank, wetting the sample by using quantitative 0.5ml-2.5ml of deionized water, uniformly mixing the water drops of the chromite sample, and adding acid to ensure that the proportion of various acids is optimal, so that the problem that a large amount of white slag powder exists at the bottom of the sample solution can be thoroughly solved after digestion.
TABLE 5 Experimental results for different amounts of DI water used for wetting
By carrying out ultrahigh pressure microwave digestion pretreatment on different chromites in countries such as Iran, Pakistan, Turkey, Aman, south Africa, Brazil, and Madagasca, and carrying out instrument and chemical analysis on the treated sample liquid, satisfactory results can be obtained.
TABLE 6 Experimental results of microwave digestion-ICP method for arsenic and lead in imported chromium ore
As can be seen from Table 6, the minimum detection result of arsenic in the chromium ore is 48. mu.g/g, and the minimum detection result of lead is 12. mu.g/g, so that the sensitivity is greatly improved.
Table 7 accuracy of chromite analysis results in units: is based on
As is clear from the analysis results in Table 7, the measured values obtained by this method match the indicated values and the measured values obtained by the conventional method.
TABLE 8 results of chromium oxide and magnesium oxide measurements from various different chromite grades by the present protocol
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A pretreatment method for putting a chromium ore into a microwave digestion acid melting method is characterized by comprising the following steps of:
firstly, weighing a chromite sample, and placing the chromite sample in a polytetrafluoroethylene digestion tank;
secondly, adding water to uniformly mix the sample, adding sulfuric acid, phosphoric acid and fluoboric acid, and covering and sleeving; placing the mixture in a turntable, placing the mixture in a microwave digestion instrument, setting parameters of an ultrahigh pressure instrument, and starting up the microwave digestion instrument;
and thirdly, after the digestion is finished, transferring the sample liquid into a bottle to be tested after the sample is cooled to room temperature.
2. The chromium ore microwave digestion acid melting method pre-treatment method according to claim 1, wherein in the first step, 0.2g of chromite ore sample is weighed and placed in a polytetrafluoroethylene digestion tank.
3. The chromium ore microwave digestion acid-melting method put into pretreatment method according to claim 1, wherein in the second step, 1.0ml of water is added to mix the sample evenly, 8ml of sulfuric acid +5ml of phosphoric acid +1ml of fluoboric acid is added, and a cover and a sleeve are added; placing in a turntable, and placing in a microwave digestion instrument.
4. The chromium ore microwave digestion acid melting method pretreatment method according to claim 1, wherein the third step sets up ultra-high pressure instrument parameters, the output power of the microwave digestion instrument is 1200W, and the temperature rise program: the time required for raising the temperature from the normal temperature to 250 ℃ under the condition of keeping 1200W of power is 30min, and the time for keeping the temperature at 250 ℃ is 40 min.
5. The method for putting the chromium ore microwave digestion acid melting method into pretreatment of the claim 1, wherein the chromium ore microwave digestion acid melting method is put into the ultrahigh pressure condition of the pretreatment method: the output power of the microwave digestion instrument is 800W-1200W, and the temperature rising program is as follows: the time required for raising the temperature from the normal temperature to 220-250 ℃ under the condition of keeping constant power is 20-35min, and the time for reaching the temperature is 25-40 min.
6. The chromium ore microwave digestion acid melting method put into pretreatment method according to claim 1, characterized in that the selection and quantification of the reagents of the chromium ore microwave digestion acid melting method put into pretreatment method: 6mL to 8mL of sulfuric acid, 4mL to 5.5mL of phosphoric acid and 0.5mL to 1.5mL of fluoroboric acid.
7. The chromium ore microwave digestion acid melting method put into pretreatment method according to claim 1, wherein the sample weight of the chromium ore microwave digestion acid melting method put into pretreatment method is 0.10g to 0.25 g.
8. The chromium ore microwave digestion acid melting method put into pretreatment method according to claim 1, characterized in that, the chromium ore microwave digestion acid melting method put into the sample of pretreatment method into the digestion tank, then wet with a quantitative 0.5ml-2.5ml of deionized water, and mix the sample water beads of chromite evenly, then add acid.
9. A ferrochromium alloy production method using the chromium ore microwave digestion acid melting method of any one of claims 1 to 8 to put into a pretreatment method.
10. A method for producing metallic chromium by using the chromium ore microwave digestion acid melting method of any one of claims 1 to 8 as a pretreatment method.
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