CN103185717A - Method for determining content of aluminum nitride in aluminum ash - Google Patents
Method for determining content of aluminum nitride in aluminum ash Download PDFInfo
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- CN103185717A CN103185717A CN2011104589882A CN201110458988A CN103185717A CN 103185717 A CN103185717 A CN 103185717A CN 2011104589882 A CN2011104589882 A CN 2011104589882A CN 201110458988 A CN201110458988 A CN 201110458988A CN 103185717 A CN103185717 A CN 103185717A
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Abstract
The invention discloses a method for measuring the content of aluminum nitride in aluminum ash. The method comprises the following steps: weighing 100-200 ml of a NaOH solution with the concentration of 20%-40%, heating the NaOH solution on a resistance furnace, adding the residual aluminum ash into a conical flask containing the NaOH solution, keeping the NaOH solution at the temperature of 80-100 DEG C, condensing ammonia produced in the conical flask, absorbing the ammonia by an absorption bottle containing a boric acid solution, keeping stirring with a magnetic stirrer, and stopping distillation after the reaction is conducted for 2-5 hours, titrating with a H2SO4 (or HCL) standard solution, with methyl red-methylene blue as an indicator, and calculating the mass fraction X1 of the nitrogen element according to the amount of consumed HCl, so that the mass fraction X of the aluminum nitride is calculated.
Description
Technical field
The present invention relates to chemical substance detection technique field, particularly aluminium nitride Determination on content method in a kind of aluminium ash.
Background technology
The aluminium ash is a kind of scum silica frost that will inevitably produce in primary aluminum or the secondary aluminium production run, is mainly derived from the oxide inclusions, flux of aluminum melt in the fusion process and carries out the material that produces behind the chemical reaction with flux; Aluminium ash principal ingredient is the oxide of metallic aluminium simple substance and aluminium oxide, aluminium nitride, villaumite and villiaumite and some other metals.Wherein, aluminium nitride is a kind of ceramics insulator, has higher heat-transfer capability, is widely used in microelectronic, can replace alumina and beryllia and be used for a large amount of electronic devices.
At present, the mensuration of aluminium ash component mainly is aluminium and the alumina content of measuring wherein, for the research of aluminium nitride assay in the aluminium ash seldom, although can adopt XRD (X-Ray Diffractomer, X-ray diffractometer) aluminium nitride content in the aluminium ash is measured, but because it is semiquantitative detection means, cannot record the accurate content of aluminium nitride, make troubles for the application of aluminium nitride.
Summary of the invention
The invention provides a kind of method of measuring aluminium nitride total amount in the aluminium ash, replenish the mensuration coverage of improving thing phase in the existing aluminium ash.
Technical scheme of the present invention is:
Aluminium nitride Determination on content method in a kind of aluminium ash may further comprise the steps:
A, measure the NaOH solution 100-200mL of 20%-40% concentration, be positioned on the resistance furnace and heat, the residual ash of aluminium ash is joined in the conical flask that NaOH solution is housed, NaOH solution is remained on 80-100 ℃;
B, the ammonia process condensation that conical flask is produced absorb ammonia with the absorption bottle that BAS is housed, and keep lasting stirring with magnetic stirring apparatus, end distillation behind the reaction 2-5h;
C, with methyl red-methylene blue as indicator, concentration known H
2SO
4(or HCl) standard solution titration, the amount that consumes according to HCl calculates the massfraction X1 of nitrogen element, can calculate the massfraction X of aluminium nitride.
Preferably, the computing formula of the massfraction X of aluminium nitride is:
X＝2.929*X1*(1-X2)
Wherein, X is the massfraction of aluminium nitride, and X1 is the massfraction of nitrogen element, and X2 is pill of aluminium massfraction, and described pill of aluminium massfraction sieves the ratio that the above alumina particles of 200 orders accounts for whole aluminium ashes for after the aluminium slag is ball milling.
Preferably, the computing formula of the massfraction X1 of nitrogen element is:
X1＝((V1-V2)*N*0.014)/m*100％
Wherein, X1 is the massfraction of nitrogen element, V1 is the volume that sample consumes sulfuric acid or salt standard acid solution, V2 is the volume that reagent blank consumes sulfuric acid or hydrochloric acid standard solution, reagent blank is the BAS in the absorption bottle, N is the N of sulfuric acid or hydrochloric acid standard solution, and 0.014 for 1N sulfuric acid or hydrochloric acid standard solution 1ml are equivalent to the nitrogen grams, and m is the residual grey quality of aluminium ash.
Preferably, before steps A, the aluminium ash is added ball mill grinding after 3 hours, again through the screening of 40 purpose screen clothes, stay the pill of aluminium that is on the screen cloth.
Preferably, among the step B, have on the conical flask of NaOH solution in condenser pipe is contained in, have under the absorption bottle liquid level of BAS in the lower end of described condenser pipe is inserted.
Preferably, among the step B, BAS is 20ml, and massfraction is 2%.
Preferably, among the step B, 1 of methyl red-methylene blue mixed indicator is housed in the described absorption bottle.
Provided by the invention, have following advantage:
1, expands the mensuration coverage of thing phase in the aluminium ash: based on the needs of aluminium ash recycling technology and to having the additional perfect of analytical approach now, proposed this assay method; This assay method is determined to be of great significance to the extraction process of aluminium nitride in the revaluation of aluminium ash economic worth and the later on possible aluminium ash;
2, measure accurately: with alkali lye and the residual ash reaction of aluminium ash, absorb the ammonia that wherein produces with BAS, thereby obtain nitrogen element content, and then calculate aluminium nitride content; By chemical analysis method aluminium nitride in the aluminium ash is accurately measured.
Embodiment
Do further detailed description below in conjunction with the technical solution of the present invention of embodiment, but embodiments of the present invention are not limited thereto.
Embodiment 1
A, measure the NaOH solution 100-200mL of 20%-40% concentration, be positioned on the resistance furnace and heat, the residual ash of aluminium ash is joined in the conical flask that NaOH solution is housed, NaOH solution is remained on 80-100 ℃, be conducive to accelerate the reaction velocity of the aluminium residual ash of ash and alkali lye.
B, the ammonia process condensation that conical flask is produced absorb ammonia with the absorption bottle that BAS is housed, and keep lasting stirring with magnetic stirring apparatus, end distillation behind the reaction 2-5h;
Have on the conical flask of NaOH solution in condenser pipe can being contained in, have under the absorption bottle liquid level of BAS in the lower end of described condenser pipe is inserted, guarantee that ammonia is all absorbed.
C, with methyl red-methylene blue as indicator, concentration known H
2SO
4(or HCl) standard solution titration, the amount that consumes according to HCl calculates the massfraction X1 of nitrogen element, can calculate the massfraction X of aluminium nitride.
Wherein, the computing formula of the massfraction X1 of nitrogen element is:
X1＝((V1-V2)*N*0.014)/m*100％ (1)
In the formula (1), X1 is the massfraction of nitrogen element, V1 is the volume that sample consumes sulfuric acid or salt standard acid solution, V2 is the volume that reagent blank consumes sulfuric acid or hydrochloric acid standard solution, reagent blank is the BAS in the absorption bottle, N is the N of sulfuric acid or hydrochloric acid standard solution, and 0.014 for 1N sulfuric acid or hydrochloric acid standard solution 1ml are equivalent to the nitrogen grams, and m is the quality of the residual ash of aluminium ash.
The computing formula of the massfraction X of aluminium nitride is:
X＝2.929*X1*(1-X2) (2)
In the formula (2), X is the massfraction of aluminium nitride, and X1 is the massfraction of nitrogen element, and X2 is pill of aluminium massfraction, and described pill of aluminium massfraction sieves the ratio that the above alumina particles of 200 orders accounts for whole aluminium ashes for after the aluminium slag is ball milling; 2.929 be atomic weight=41/14 of AlN atomic weight/N.The pill of aluminium can obtain by following method: the aluminium ash was added ball mill grinding after 3 hours, again through the screening of 40 purpose screen clothes, stay the pill of aluminium that is on the screen cloth, under the screen cloth is aluminium ash residual ash, i.e. reactant in the steps A.
Embodiment 2
In bowl mill, add the aluminium ash, grind after 3 hours, through 40 purpose screen clothes, sieve out the oarse-grained pill of aluminium, calculate the massfraction X2 of the pill of aluminium; And the residual ash of remaining aluminium ash carried out chemical analysis: put into the NaOH solution 100-200mL of 20%-40% concentration with the grey residual grey mg aluminium ash of ten thousand/balance weighing aluminium, cover tightly bottle stopper rapidly, be positioned on the resistance furnace then and heat, maintain the temperature at 80-100 ℃.The ammonia that produces in the bottle enters in the receiving bottle that 1 of 20ml 2% BAS and methyl red-methylene blue mixed indicator is housed through condenser pipe (insert under the receiving bottle liquid level lower end of condenser pipe), allows its reaction 3h.Take off receiving bottle, fixed with the 0.01N sulfuric acid droplets is terminal point to grey or with the molten titration of 0.01N hydrochloric acid standard to bluish violet, and record consumes the volume V1 ml of sulfuric acid or salt standard acid solution.
Draw 20.0ml 2% BAS simultaneously and carry out titration operation as reagent blank, fixed with the 0.01N sulfuric acid droplets equally is terminal point to grey or with the molten titration of 0.01N hydrochloric acid standard to bluish violet, the sulfuric acid that record consumes or the volume V2 ml of hydrochloric acid standard solution.
Calculate according to the formula among the embodiment 1 (1) and formula (2) then, namely obtain the massfraction of aluminium nitride.
More than in a kind of aluminium ash that the embodiment of the invention is provided aluminium nitride Determination on content method be described in detail, used specific case herein principle of the present invention and embodiment set forth, only be used for helping to understand core concept of the present invention; Should not be construed as limitation of the present invention.
Claims (7)
1. aluminium nitride Determination on content method in the aluminium ash is characterized in that, may further comprise the steps:
A, measure the NaOH solution 100-200mL of 20%-40% concentration, be positioned on the resistance furnace and heat, the residual ash of aluminium ash is joined in the conical flask that NaOH solution is housed, NaOH solution is remained on 80-100 ℃;
B, the ammonia process condensation that conical flask is produced absorb ammonia with the absorption bottle that BAS is housed, and keep lasting stirring with magnetic stirring apparatus, end distillation behind the reaction 2-5h;
C, with methyl red-methylene blue as indicator, concentration known H
2SO
4(or HCl) standard solution titration, the amount that consumes according to HCl calculates the massfraction X1 of nitrogen element, can calculate the massfraction X of aluminium nitride.
2. aluminium nitride Determination on content method in a kind of aluminium ash according to claim 1 is characterized in that the computing formula of the massfraction X of aluminium nitride is:
X＝2.929*X1*(1-X2)
Wherein, X is the massfraction of aluminium nitride, and X1 is the massfraction of nitrogen element, and X2 is pill of aluminium massfraction, and described pill of aluminium massfraction sieves the ratio that the above alumina particles of 200 orders accounts for whole aluminium ashes for after the aluminium slag is ball milling.
3. aluminium nitride Determination on content method in a kind of aluminium ash according to claim 2 is characterized in that the computing formula of the massfraction X1 of nitrogen element is:
X1＝((V1-V2)*N*0.014)/m*100％
Wherein, X1 is the massfraction of nitrogen element, V1 is the volume that sample consumes sulfuric acid or salt standard acid solution, V2 is the volume that reagent blank consumes sulfuric acid or hydrochloric acid standard solution, reagent blank is the BAS in the absorption bottle, N is the N of sulfuric acid or hydrochloric acid standard solution, and 0.014 for 1N sulfuric acid or hydrochloric acid standard solution 1ml are equivalent to the nitrogen grams, and m is the residual grey quality of aluminium ash.
4. aluminium nitride Determination on content method in a kind of aluminium ash according to claim 2 is characterized in that, before steps A, the aluminium ash is added ball mill grinding after 3 hours, again through the screening of 40 purpose screen clothes, stays the pill of aluminium that is on the screen cloth.
5. according to aluminium nitride Determination on content method in each described a kind of aluminium ash of claim 1 to 4, it is characterized in that, among the step B, have on the conical flask of NaOH solution in condenser pipe is contained in, have under the absorption bottle liquid level of BAS in the lower end of described condenser pipe is inserted.
6. according to aluminium nitride Determination on content method in each described a kind of aluminium ash of claim 1 to 4, it is characterized in that among the step B, BAS is 20ml, massfraction is 2%.
7. according to aluminium nitride Determination on content method in each described a kind of aluminium ash of claim 1 to 4, it is characterized in that, among the step B, 1 of methyl red-methylene blue mixed indicator is housed in the described absorption bottle.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103399011A (en) * | 2013-08-22 | 2013-11-20 | 重庆紫光化工股份有限公司 | Measuring method of content of cyanoacetic acid product |
| CN104062396A (en) * | 2014-07-14 | 2014-09-24 | 四川天齐锂业股份有限公司 | Method for measuring content of nitrogen in metal lithium and lithium alloy |
| CN105347361A (en) * | 2015-11-20 | 2016-02-24 | 陈湘清 | Comprehensive utilization method of aluminum ash |
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| CN102087208A (en) * | 2010-12-21 | 2011-06-08 | 湖南晟通科技集团有限公司 | Method for detecting content of oxide inclusion in aluminium and aluminium alloys |
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2011
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| JPH01138457A (en) * | 1987-11-25 | 1989-05-31 | Denki Kagaku Kogyo Kk | Nitrogen compound decomposing agent and quantitative analysis of nitrogen in nitrogen compound |
| CN101178393A (en) * | 2007-11-30 | 2008-05-14 | 莱芜钢铁集团有限公司 | Device for accurately determining trace quantity nitrogen in alloy or metal |
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| CN103399011A (en) * | 2013-08-22 | 2013-11-20 | 重庆紫光化工股份有限公司 | Measuring method of content of cyanoacetic acid product |
| CN104062396A (en) * | 2014-07-14 | 2014-09-24 | 四川天齐锂业股份有限公司 | Method for measuring content of nitrogen in metal lithium and lithium alloy |
| CN105347361A (en) * | 2015-11-20 | 2016-02-24 | 陈湘清 | Comprehensive utilization method of aluminum ash |
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Address after: Sheng Tong Industrial Park No. 109 Venus Road 410200 in Hunan province Changsha District of Wangcheng City Applicant after: Suntown Technology Group Corporation Address before: Sheng Tong Industrial Park No. 109 Venus Road 410200 in Hunan province Changsha District of Wangcheng City Applicant before: Hunan Shengtong Technology Group Co., Ltd. |
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