CN114436317B - Regeneration method of rare earth copper oxide for nitrogen-oxygen analyzer in ferroalloy nitrogen-oxygen analysis - Google Patents
Regeneration method of rare earth copper oxide for nitrogen-oxygen analyzer in ferroalloy nitrogen-oxygen analysis Download PDFInfo
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- CN114436317B CN114436317B CN202210062219.9A CN202210062219A CN114436317B CN 114436317 B CN114436317 B CN 114436317B CN 202210062219 A CN202210062219 A CN 202210062219A CN 114436317 B CN114436317 B CN 114436317B
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- rare earth
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- nitrogen
- oxygen
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- 239000005751 Copper oxide Substances 0.000 title claims abstract description 78
- 229910000431 copper oxide Inorganic materials 0.000 title claims abstract description 78
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 75
- -1 rare earth copper oxide Chemical class 0.000 title claims abstract description 71
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000004458 analytical method Methods 0.000 title claims abstract description 23
- 229910001021 Ferroalloy Inorganic materials 0.000 title claims abstract description 16
- 238000011069 regeneration method Methods 0.000 title description 7
- 239000000919 ceramic Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 17
- 230000001172 regenerating effect Effects 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 15
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 229910000882 Ca alloy Inorganic materials 0.000 claims description 11
- 229910001199 N alloy Inorganic materials 0.000 claims description 11
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 claims description 11
- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 claims description 11
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 6
- 239000010421 standard material Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 150000002910 rare earth metals Chemical group 0.000 claims description 5
- 238000001514 detection method Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 8
- 238000005485 electric heating Methods 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000000357 thermal conductivity detection Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/202—Constituents thereof
- G01N33/2022—Non-metallic constituents
Abstract
The invention relates to a method for regenerating rare earth copper oxide for a nitrogen-oxygen analyzer in ferroalloy nitrogen-oxygen analysis, which comprises the following steps: uniformly spreading 40-50g of inactive rare earth copper oxide in a ceramic square boat, and heating the ceramic square boat on an electric heating plate; when the rare earth copper oxide is completely changed into black gray, the ceramic ark carrying the rare earth copper oxide is placed in a dryer for natural cooling, and then the regenerated rare earth copper oxide is obtained and stored. The method re-achieves the effect of the rare earth copper oxide in the nitrogen-oxygen analysis process after high-temperature oxidation of the reduced rare earth copper oxide. The rare earth copper oxide is regenerated with the lowest cost and simple operation, and the regenerated rare earth copper oxide has good use effect and can meet the analysis and detection requirements. Resource waste is avoided, and detection cost is effectively saved. The rare earth copper oxide for monthly detection can save purchasing cost by ten thousand yuan, and the purchasing cost of the rare earth copper oxide can be saved by more than one hundred thousand yuan in a year.
Description
Technical Field
The invention relates to the technical field of rare earth copper oxide regeneration, in particular to a method for regenerating rare earth copper oxide in a nitrogen-oxygen analyzer during nitrogen-oxygen detection of ferroalloy.
Background
The nitrogen-oxygen analyzer is widely used for analyzing the nitrogen-oxygen content in ferrous metals, nonferrous metals and alloys thereof, hard alloys, inorganic materials, inorganic oxides, ferroalloys, rare earth metals and the like. In analyzing the sample, the sample is weighed and placed in the sample port and then rinsed with a carrier gas to prevent the entry of atmospheric air into the furnace system. The graphite crucible is degassed in a pulse furnace to minimize self-contained contamination. After the stabilization phase the sample falls into a crucible and melts. Oxygen in the sample reacts with carbon in the graphite crucible to form carbon monoxide. Nitrogen is released in elemental form. The carrier gas (such as helium) and the sample gas pass through the dust filter screen and then enter the rare earth copper oxide catalytic furnace to oxidize carbon monoxide into carbon dioxide. Carbon dioxide enters an infrared cell for measuring the oxygen content, the measured gas is led into a chemical reagent tube, at the moment, the carbon dioxide and the water are removed by the chemical reagent, and the nitrogen element is measured through the thermal conductivity detection cell.
The rare earth copper oxide is copper oxide extracted from rare earth, is +2 oxide of copper, can lose efficacy due to reduction of carbon monoxide after being used for a period of time, and can be tested after being replaced. Rare earth copper oxide is expensive and has high detection cost.
After rare earth copper oxide used in the nitrogen-oxygen analysis process of the iron alloy is used for a period of time, the iron alloy can be disabled due to reduction of carbon monoxide, and the iron alloy can be tested after being replaced. The regeneration technology of rare earth-free copper oxide is searched. In order to solve the problem, a rare earth copper oxide regeneration method for detecting the ferroalloy in a nitrogen-oxygen analyzer is developed.
Disclosure of Invention
The invention aims to avoid the defects of the prior art and provides a method for regenerating rare earth copper oxide for a nitrogen oxide analyzer in nitrogen oxide analysis of an iron alloy, which is used for repeatedly detecting and utilizing the rare earth copper oxide in the nitrogen oxide analyzer for the iron alloy.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a method for regenerating rare earth copper oxide for a nitrogen-oxygen analyzer in ferroalloy nitrogen-oxygen analysis comprises the following steps:
Step one, collecting 40-50g of rare earth copper oxide which is used by the ferroalloy nitrogen-oxygen analyzer and has been deteriorated and deactivated;
Uniformly spreading the collected rare earth copper oxide in a ceramic square boat with the area size of the bottom surface of 50mm multiplied by 90mm to 60mm multiplied by 110mm according to the thickness of 2mm to 3mm, wherein the thickness of the bottom surface of the ceramic square boat is less than 3mm, and then placing the ceramic square boat on an electric heating plate at 400-450 ℃ for heating for 3.5-4 hours;
When the rare earth copper oxide is completely changed into black gray, naturally cooling the ceramic ark bearing the rare earth copper oxide in a dryer, and enabling the temperature of the rare earth copper oxide and the ceramic ark to reach 23-28 ℃ within 1 hour to obtain the regenerated rare earth copper oxide;
and fourthly, placing the obtained regenerated rare earth copper oxide in a brown glass bottle for preservation.
Further, the method also comprises a step five of verifying the regeneration effect of the rare earth copper oxide by using an iron alloy standard substance:
Using the regenerated rare earth copper oxide obtained in the step three to respectively determine the oxygen content of the standard substances of the silicon-calcium alloy or the vanadium-nitrogen alloy in the ferroalloy nitrogen-oxygen analyzer;
And compared with the oxygen content value provided by the standard material evidence of the silicon-calcium alloy or the vanadium-nitrogen alloy, the deviation of the oxygen content of the standard material of the silicon-calcium alloy or the vanadium-nitrogen alloy, which is actually measured, is smaller than or equal to the repeatability limit or the allowable difference specified by the corresponding national standard or line standard analysis method, so that the regenerated rare earth copper oxide can be verified to meet the analysis requirement of the iron alloy nitrogen-oxygen analyzer.
Further, 50-60 g of regenerated rare earth copper oxide is contained in the brown glass bottle in the step four.
Further, in the second step, the collected rare earth copper oxide is uniformly paved in a ceramic square boat with the bottom surface area size of 60mm multiplied by 90mm according to the thickness of 2 mm-3 mm, the bottom surface thickness of the ceramic square boat is 2.3mm, and then the ceramic square boat is placed on an electric heating plate at 450 ℃ for heating for 4 hours.
Furthermore, the ceramic ark is a rectangular or square groove body made of ceramics. The ceramic ark is a mature product and is easy to obtain in the market.
The beneficial effects of the invention are as follows: the method re-achieves the effect of the rare earth copper oxide in the nitrogen-oxygen analysis process of the ferroalloy after high-temperature oxidation of the reduced rare earth copper oxide. The rare earth copper oxide is regenerated with the lowest cost and simple operation, and the regenerated rare earth copper oxide has good use effect and can meet the analysis and detection requirements. Resource waste is avoided, and detection cost is effectively saved. The rare earth copper oxide for monthly detection can save purchasing cost by ten thousand yuan, and the purchasing cost of the rare earth copper oxide can be saved by more than one hundred thousand yuan in a year.
Detailed Description
The principles and features of the present invention are described below with examples given for the purpose of illustration only and are not intended to limit the scope of the invention.
Example 1: a method for regenerating rare earth copper oxide for a nitrogen-oxygen analyzer in ferroalloy nitrogen-oxygen analysis comprises the following steps:
Step one, collecting 40-50g of rare earth copper oxide which is used by the ferroalloy nitrogen-oxygen analyzer and has been deteriorated and deactivated;
Uniformly spreading the collected rare earth copper oxide in a ceramic square boat with the area size of the bottom surface of 50mm multiplied by 90mm to 60mm multiplied by 110mm according to the thickness of 2mm to 3mm, wherein the thickness of the bottom surface of the ceramic square boat is less than 3mm, and then placing the ceramic square boat on an electric heating plate at 400-450 ℃ for heating for 3.5-4 hours; the ceramic ark is a rectangular or square groove body made of ceramics.
When the rare earth copper oxide is completely changed into black gray, naturally cooling the ceramic ark bearing the rare earth copper oxide in a dryer, and enabling the temperature of the rare earth copper oxide and the ceramic ark to reach 23-28 ℃ within 1 hour to obtain the regenerated rare earth copper oxide;
And fourthly, placing the obtained regenerated rare earth copper oxide in a brown glass bottle for preservation. The brown glass bottle contains 50-60 g of regenerated rare earth copper oxide.
Fifthly, verifying the regeneration effect of the rare earth copper oxide by using an iron alloy standard substance: using the regenerated rare earth copper oxide obtained in the third step to respectively determine the oxygen content of the standard substances of the silicon-calcium alloy or the vanadium-nitrogen alloy in the iron alloy nitrogen-oxygen analyzer;
And compared with the oxygen content value provided by the standard material evidence of the silicon-calcium alloy or the vanadium-nitrogen alloy, the deviation of the oxygen content of the standard material of the silicon-calcium alloy or the vanadium-nitrogen alloy, which is actually measured, is smaller than or equal to the repeatability limit or the allowable difference specified by the corresponding national standard or line standard analysis method, so that the regenerated rare earth copper oxide can be verified to meet the analysis requirement of the iron alloy nitrogen-oxygen analyzer.
If the vanadium-nitrogen alloy is used for verification, the analysis deviation is smaller than or equal to the precision requirement specified in GB/T24583.7-2019 "infrared absorption method for measuring the oxygen content of vanadium-nitrogen alloy", the following table is provided:
| oxygen content% (mass fraction) | Limit% of repeatability r |
| 0.10～0.50 | 0.02 |
| >0.50～1.00 | 0.04 |
| >1.00～2.00 | 0.06 |
| >2.00～4.00 | 0.08 |
If the silicon-calcium alloy is used for verification, the analysis deviation is less than or equal to the allowable difference requirement specified in YB/T4738-2019 inert gas melting infrared absorption method for measuring oxygen content of silicon-calcium alloy, and the following table is provided:
When the ferroalloy is subjected to nitrogen-oxygen analysis, after one third of rare earth copper oxide is reduced to red in an oxidation furnace and a purification furnace of a nitrogen-oxygen analyzer, the catalytic effect is poor, the ferroalloy should be replaced by new or regenerated rare earth copper oxide, the copper oxide content in the required rare earth copper oxide is detected to be more than 70%, and the copper oxide content in the regenerated rare earth copper oxide is more than 90%, so that the effect is remarkable.
Example 2: in the same manner as in example 1, except that the collected rare earth copper oxide was uniformly spread in a ceramic ark having a bottom surface area size of 60mm×90mm at a thickness of 2mm to 3mm, the bottom surface thickness of the ceramic ark was 2.3mm, and then, the ceramic ark was heated on a hot plate at 450 ℃ for 4 hours. By adopting the scheme of the embodiment, the content of copper oxide in the regenerated rare earth copper oxide reaches 95 percent and is far beyond the use standard, so the invention adopts low-cost and simple method steps and achieves unexpected technical effects.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (3)
1. The method for regenerating the rare earth copper oxide for the nitrogen-oxygen analyzer in the nitrogen-oxygen analysis of the ferroalloy is characterized by comprising the following steps of:
Step one, collecting 40-50g of rare earth copper oxide which is used by the ferroalloy nitrogen-oxygen analyzer and has been deteriorated and deactivated;
Uniformly paving the collected rare earth copper oxide in a ceramic square boat with the bottom surface area size of 60mm multiplied by 90mm according to the thickness of 2 mm-3 mm, wherein the bottom surface thickness of the ceramic square boat is 2.3mm, and then heating the ceramic square boat on an electric plate at 450 ℃ for 4 hours;
When the rare earth copper oxide is completely changed into black gray, naturally cooling the ceramic ark bearing the rare earth copper oxide in a dryer, and enabling the temperature of the rare earth copper oxide and the ceramic ark to reach 23-28 ℃ within 1 hour to obtain the regenerated rare earth copper oxide;
Fourthly, placing the obtained regenerated rare earth copper oxide into a brown glass bottle for storage; the brown glass bottle contains 50-60 g of regenerated rare earth copper oxide.
2. The method for regenerating a rare earth copper oxide for a nitrogen oxide analyzer in a nitrogen oxide analysis of an iron alloy according to claim 1, further comprising a step of verifying a regenerating effect of the rare earth copper oxide by using an iron alloy standard substance:
Using the regenerated rare earth copper oxide obtained in the three steps to respectively determine the oxygen content of the silicon-calcium alloy or vanadium-nitrogen alloy standard substance in the iron alloy nitrogen-oxygen analyzer;
And compared with the oxygen content value provided by the standard material evidence of the silicon-calcium alloy or the vanadium-nitrogen alloy, the deviation of the oxygen content of the standard material of the silicon-calcium alloy or the vanadium-nitrogen alloy, which is actually measured, is smaller than or equal to the repeatability limit or the allowable difference specified by the corresponding national standard or line standard analysis method, so that the regenerated rare earth copper oxide can be verified to meet the analysis requirement of the iron alloy nitrogen-oxygen analyzer.
3. The method for regenerating rare earth copper oxide for a nitrogen-oxygen analyzer in nitrogen-oxygen analysis of an iron alloy according to claim 1 or 2, wherein the ceramic ark is a rectangular or square groove body made of ceramics.
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| Application Number | Priority Date | Filing Date | Title |
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| CN114436317A CN114436317A (en) | 2022-05-06 |
| CN114436317B true CN114436317B (en) | 2024-04-30 |
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- 2022-01-19 CN CN202210062219.9A patent/CN114436317B/en active Active
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