CN103091200A - Method and device for detecting metal aluminum content in burned ash - Google Patents

Method and device for detecting metal aluminum content in burned ash Download PDF

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CN103091200A
CN103091200A CN2012105917145A CN201210591714A CN103091200A CN 103091200 A CN103091200 A CN 103091200A CN 2012105917145 A CN2012105917145 A CN 2012105917145A CN 201210591714 A CN201210591714 A CN 201210591714A CN 103091200 A CN103091200 A CN 103091200A
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volume
glass vessel
graduated cylinder
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glassware
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CN103091200B (en
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胡艳军
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Guangdong Gaohang Intellectual Property Operation Co ltd
Zhejiang Haining Warp Knitting Industrial Park Development Co.,Ltd.
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Zhejiang University of Technology ZJUT
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Abstract

The invention discloses a method and a device for detecting metal aluminum content in burned ash. The method comprises the following steps of placing a burned ash sample into a small-opening glass vessel with a magnetic stirring stick, then placing the burned ash sample into a large-opening glass vessel, reversely arranging a measuring cylinder and covering the small-opening glass vessel, perforating the bottom of the measuring cylinder, and sealing a hole in the bottom of the measuring cylinder by a rubber leather pad and glue; pouring a sodium hydroxide solution with the concentration of 4 to 5 percent into the large-opening glass vessel, inserting a head of an air needle into the small hole which is formed in the bottom of the measuring cylinder and stuck with the rubber leather pad, and extracting air; performing heating and stirring reaction, recording a liquid level height value of the solution in the measuring cylinder until the liquid level height is not changed, and recording the volume V1 corresponding to the final liquid level height; and calculating the volume of hydrogen according to a volume difference, and calculating the mass percentage of metal aluminum and the mass percentage of the metal aluminum in the burned ash. The invention provides the simple and quick method for precisely measuring the metal aluminum content in the burned ash; the method is easy to operate and execute; a requirement on a device is low; an alkaline solution reagent can be repeatedly used; and the accuracy is high.

Description

A kind of method and device that detects metallic aluminium content in burning ash
Technical field
The present invention relates to the technical field of metallic aluminium content detection in thin material, especially for comprise the higher domestic waste of aluminum waste content, industrial refuse, medical waste flying ash that burning produces afterwards and grain diameter less than the incineration bottom ash of 2mm in the metal aluminum content tests.
Background technology
Economic fast development, quickening and the commercial production of urbanization process progressively make the transition, make all kinds of municipal refuses comprise the output increase year after year of domestic waste, medical waste, industrial refuse, great variety had also occured with past 10 years in the physics component, wherein, in these rubbish, the content of scrap metal pieces is particularly remarkable.Due to metallic aluminium aboundresources, cheap and easy characteristics such as plastotype, in daily life with commercial production in use amount larger.In house refuse, the metallic aluminium waste content is risen to now 0.4% by less than 0.02% before 10 years, mainly comprises aluminium ring pull end, In Aluminium Foil Packing goods; In addition, in medical product, the easily-consumed products of aluminum, medicine packing etc. also are used widely; In commercial production, the tailing generation of aluminum products is also a lot.Yet, usually these waste products not in time classification reclaim, wherein a part directly or with domestic garbage mixing is delivered to burning electricity generation factory and office reason.
The ratio that the Chinese large-sized municipal refuse adopts incineration technology to process rises year by year, and the house refuse of burning disposal accounts for total product rubbish 8% at present.Expect 2015, the incineration treatment of garbage ratio of some large size cities will increase more than 20%.The accessory substance burning ash of waste incineration comprises flying dust and bottom ash, along with the thinking of solid waste recycling treatment is widelyd popularize, these two kinds of ashes are applied to building materials and roadbed material usually, and the thinking of this recycling treatment burning accessory substance has obtained the promotion energetically of Government and enterprise.Present flying ash and bottom ash aggregate are produced as the ecological architectural material products such as cement, space brick day by day to be increased, and is subject to all circles' favorable comment.
Yet the shortcoming such as fracture, foaming usually in use appear in the ecological architectural material that incinerator ash transforms, compressive strength is poor, Nian Jiuyi is broken causes these ecomaterials can not obtain the application of higher level.One of reason is exactly that complicated incinerator ash physics component causes, such as comprising the packaging wastes such as a small amount of aluminum products in different types of rubbish, oxidation on metal surface generates fine and close oxide and has stoped the continuation oxidation of other metallic aluminium in the high temperature incineration process, and the metallic aluminium after burning enters in flying dust or bottom ash according to the pattern of incinerator.In alkaline environment, the chemical reaction as shown in (1), (2), (3) can occur in the metallic aluminium generation that the lime-ash regeneration aggregate comprises.Al (OH) due to both sexes 3Water-soluble, and at PH〉can not form purification layer in 10 strong alkali solution, the themopositive reaction of aluminium and water generates aluminate ion; If environment alkalescence is reduced to pH=9-10, aluminate ion decomposites Al (OH) again 3In case, Al (OH) 3Lower than solubility product, it will produce the gelinite precipitation; Simultaneously, according to chemical equation (4), due to Al (OH) 3With the generation of aluminate, both produce new sediment [CaAl (OH) in alkaline environment 6] 2, these sediments are to cause ecological architectural material in use to produce one of the reason in crack.Be confirmed in this point academic documents abroad.
Figure BDA0000268418281
(1)
(2)
(3)
Figure BDA0000268418284
(4)
Present Domestic is the apparatus and method of aluminium content detection in relevant thin material also.If can just grasp the wherein content situation of metallic aluminium before the incinerator ash resource is used, for the optimization of combustion ash be converted into the pretreatment technology of high-quality ecological architectural material, the engineering characteristic etc. that improves burning ash has important directive significance and realistic price, also the lime-ash purified treatment is improved Useful Information.
Summary of the invention
The invention provides the method for metallic aluminium content in a kind of easy, quick, Accurate Measurement burning ash, can be fast, accurately be the mass concentration that hydrogen volume that in 4 ~ 5% sodium hydroxide solution and burning ash, metallic aluminium generation chemical reaction produces calculates metallic aluminium in ash discharge by concentration.The method is simple to operate, easy enforcement, low to matching requirements, save reagent, accuracy rate is high.
The technical solution used in the present invention is:
A kind of method that detects metallic aluminium content in burning ash, said method comprising the steps of: (1) is weighing burning ash sample accurately, quality is M g, the burning ash sample after weighing is positioned in little open glass vessel, and places magnetic stirring bar in little open glass vessel; The little open glass vessel that burning ash sample and magnetic stirring bar are housed are placed in the big open end glassware volume V of big open end glassware bThe volume V of mL and little open glass vessel sThe ratio of mL is the preferred 15-50:1 of 15-100:1(); Foraminate graduated cylinder is opened in one bottom stand upside down, cover the little open glass vessel in the big open end glassware, the volume V of graduated cylinder 0ML, V b– V 0>0, the aperture of graduated cylinder bottom is with rubber pad and glue hermetic seal aperture;
(2) be that the sodium hydroxide solution of 4 ~ 5% (preferred 5%) is poured in the big open end glassware with mass concentration, the volume of sodium hydroxide solution is V NaOH, and V 0<V NaOH<V bThe air tube syringe needle that one end is connected aspiration pump inserts the aperture that the graduated cylinder bottom that covers little open glass vessel of standing upside down is stained with rubber pad, starts the aspiration pump air in graduated cylinder of finding time, and makes to be full of sodium hydroxide solution in graduated cylinder fully, takes out the air tube syringe needle; Start magnetic agitation, with the heating of big open end glassware, the temperature of controlling solution in the big open end glassware is 45 ~ 55 ℃ (preferred 50 ℃), begins reaction;
(3) liquid level of solution height in the time recording graduated cylinder, until liquid level is constant, record volume V corresponding to last liquid level 1Calculate hydrogen volume=(V 0-V 1) mL; The burning ash Gold Samples belongs to the quality of aluminium=(V 0-V 1) * 0.8036 * 10 -3g
The burning ash Gold Samples belongs to the mass percentage concentration of aluminium=[(V 0-V 1) * 0.8036 * 10 -3/ M] * 100%.
Described big open end glassware volume V b, the graduated cylinder volume V 0, sodium hydroxide solution volume V NaOHSatisfy following relation:
(1/10)V b≤(V NaOH- V 0)<(V b –V 0)
Burning ash of the present invention is the accessory substance of waste incineration, can be flying dust or bottom ash.Burning ash can directly obtain from garbage burning factory.
The diameter of graduated cylinder small hole at bottom part of the present invention is preferably less than 0.5cm.
Described big open end glassware is preferably large beaker, and described little open glass vessel are preferably small beaker.
The present invention also provides a kind of device that detects metallic aluminium content in burning ash, described device comprises the big open end glassware, is positioned over the little open glass vessel of the burning ash the placed sample in the big open end glassware, the graduated cylinder of bottom perforate, and an end connects the air tube syringe needle of aspiration pump; Be placed with magnetic stirring bar in described little open glass vessel; The graduated cylinder of bottom perforate is inverted, and covers the little open glass vessel in the big open end glassware, the aperture rubber pad hermetic seal of graduated cylinder bottom; Described big open end glassware is positioned on the well heater of temp. controllable, and is provided with thermometer in described big open end glassware, and described well heater has magnetic stirring function.
Described big open end glassware is preferably large beaker, and described little open glass vessel are preferably small beaker.
In described device, the volume V of preferred described big open end glassware bThe volume V of mL and little open glass vessel sThe ratio of mL is 15-100:1, preferred 15-50:1;
The volume of described graduated cylinder is V 0ML, and satisfy V b– V 0>0.
Design theory of the present invention is:
In burning ash, the theoretical foundation of metallic aluminium assay is chemical reaction to occur in alkaline environment (PH=12-14) according to metallic aluminium produce hydrogen, go out the quality of metallic aluminium according to the hydrogen volume of collecting (ml) backwards calculation, and then calculate the mass percent of metallic aluminium in burning ash.The chemical equation that metallic aluminium occurs in alkaline solution is:
2Al + 6H 2O +2NaOH > 2NaAl(OH) 4 + 3H 2
The operation steps of described step (2) should be completed as early as possible, to prevent that Gold Samples from belonging to aluminium and react and in time do not collect the hydrogen of generation in alkaline solution.
In described step (3), usually recorded the liquid level value of solution in graduated cylinder every 20 minutes, record until liquid level till the numerical value of continuous three times is constant, obtaining last liquid level value is V 1
Beneficial effect of the present invention is mainly manifested in: the method can be easy, detect fast and accurately-calculate the mass concentration of metallic aluminium in burning ash or relevant thin material.The temperature of reaction of having verified by experiment solution keeps continuing under stirring condition at 50 ℃ of left and right, alkaline PH=12-14 and sample and solution, the reaction velocity of metallic aluminium is faster, reaction more thorough.The method can be accomplished to seal preferably and to the preservation of hydrogen, be carried out aforesaid operations by the thin slice aluminium foil (aluminium content 97%) to certain mass, has verified that the method reaches more than 99.8% the detection of metallic aluminium is efficient.The method of metallic aluminium content in detection burning ash provided by the invention, simple to operate, easy enforcement, low to matching requirements, alkaline reagent solution is reusable, accuracy rate is high.
Description of drawings:
Fig. 1 detects the schematic diagram of the device of metallic aluminium content in burning ash.
Fig. 2 detects the process flow diagram of the method for metallic aluminium content in burning ash.
Embodiment
The present invention will be further described with specific embodiment for the below, but protection scope of the present invention is not limited to this.
Embodiment 1
The 1 couple of the present invention device that detects metallic aluminium content in burning ash describes by reference to the accompanying drawings, and Fig. 1 is a kind of optimal way of the present invention's device of detecting metallic aluminium content in burning ash.In described detection burning ash, the device of metallic aluminium content comprises large beaker 1, is positioned over the air tube syringe needle that placing in large beaker 1 put graduated cylinder 3, the one ends connection aspiration pumps of the small beaker 2 of burning ash sample, bottom perforate; Be placed with magnetic stirring bar 9 in described small beaker 2; The graduated cylinder 3 of bottom perforate is inverted, and covers the small beaker 2 in large beaker 1, and the aperture of graduated cylinder bottom is with rubber pad 4 hermetic seals; Described large beaker 1 is positioned on the well heater 5 of temp. controllable, and is provided with thermometer 8 in described large beaker 1, and described well heater 5 has magnetic stirring function.On well heater 5, be provided with temperature controller 6 and magnetic stirring speed regulator 7.
Concrete operation step is:
(1) accurate weighing one small pieces aluminium foil (metallic aluminium content is 97%, and other is magnesium, copper etc.), quality is 0.5g, the foil samples after weighing is positioned in the small beaker of 20mL, and places magnetic stirring bar in small beaker; The small beaker that foil samples and magnetic stirring bar are housed is placed in the large beaker of 1000mL, foraminate graduated cylinder is opened in a bottom stand upside down, cover the small beaker in large beaker, the volume V of graduated cylinder 0=800mL, the hole diameter 0.35cm of graduated cylinder bottom is with rubber pad and glue hermetic seal aperture;
(2) be that 5% sodium hydroxide solution is poured in large beaker with mass concentration, the volume of sodium hydroxide solution is 900mL.The air tube syringe needle that one end is connected aspiration pump inserts the aperture that the graduated cylinder bottom that covers small beaker of standing upside down is stained with rubber pad, starts the aspiration pump air in graduated cylinder of finding time, and makes to be full of sodium hydroxide solution in graduated cylinder fully, takes out the air tube syringe needle; Start magnetic agitation, with the large beaker heating, the temperature of controlling solution in large beaker is 50 ℃, begins reaction;
(3) recorded the liquid level height value of solution in graduated cylinder every 20 minutes, when continuous liquid level of measuring cylinder value does not all change in continuous three measurements, volume V corresponding to last liquid level recorded in stopped heating and stirring 1=200 mL; Calculate hydrogen volume=600 mL; The burning ash Gold Samples belongs to the quality of aluminium=(V 0-V 1) * 0.8036 * 10 -3G=0.482g
In selected foil samples, the quality of containing metal aluminium is=0.485 g.Test result and actual value only differ from 0.6%
Embodiment 2
Concrete operation step is:
(1) (metallic aluminium content is 97% for the fine sand material (can cross the standard sieve of 2mm) of accurate weighing 2g natural recovery for building and a small pieces aluminium foil, other is magnesium, copper etc.), quality is 0.27g, aluminium foil after weighing is buried in fine sand, then be positioned in the small beaker of 20mL, and place magnetic stirring bar in small beaker; The small beaker that fine sand, aluminium foil and magnetic stirring bar are housed is placed in the large beaker of 1000mL, foraminate graduated cylinder is opened in a bottom stand upside down, cover the small beaker in large beaker, the volume V of graduated cylinder 0=800mL, the hole diameter 0.35cm of graduated cylinder bottom is with rubber pad and glue hermetic seal aperture;
(2) be that 5% sodium hydroxide solution is poured in large beaker with mass concentration, the volume of sodium hydroxide solution is 900mL.The air tube syringe needle that one end is connected aspiration pump inserts the aperture that the graduated cylinder bottom that covers small beaker of standing upside down is stained with rubber pad, starts the aspiration pump air in graduated cylinder of finding time, and makes to be full of sodium hydroxide solution in graduated cylinder fully, takes out the air tube syringe needle; Start magnetic agitation, with the large beaker heating, the temperature of controlling solution in large beaker is 50 ℃, begins reaction;
(3) recorded the liquid level height value of solution in graduated cylinder every 20 minutes, when continuous liquid level of measuring cylinder value does not all change in continuous three measurements, volume V corresponding to last liquid level recorded in stopped heating and stirring 1=475 mL; Calculate hydrogen volume=325 mL; The burning ash Gold Samples belongs to the quality of aluminium=(V 0-V 1) * 0.8036 * 10 -3G=0.261 g
In selected foil samples, the quality of containing metal aluminium is=0.262 g.Test result and actual value only differ from 0.038%.

Claims (8)

1. method that detects metallic aluminium content in burning ash, it is characterized in that said method comprising the steps of: (1) is weighing burning ash sample accurately, quality is M g, burning ash sample after weighing is positioned in little open glass vessel, and places magnetic stirring bar in little open glass vessel; The little open glass vessel that burning ash sample and magnetic stirring bar are housed are placed in the big open end glassware volume V of big open end glassware bThe volume V of mL and little open glass vessel sThe ratio of mL is 15-100:1; Foraminate graduated cylinder is opened in one bottom stand upside down, cover the little open glass vessel in the big open end glassware, the volume V of graduated cylinder 0ML, V b– V 0>0, the aperture of graduated cylinder bottom is with rubber pad and glue hermetic seal aperture;
(2) be that 4 ~ 5% sodium hydroxide solution is poured in the big open end glassware with mass concentration, the volume of sodium hydroxide solution is V NaOH, and V 0<V NaOH<V bThe air tube syringe needle that one end is connected aspiration pump inserts the aperture that the graduated cylinder bottom that covers little open glass vessel of standing upside down is stained with rubber pad, starts the aspiration pump air in graduated cylinder of finding time, and makes to be full of sodium hydroxide solution in graduated cylinder fully, takes out the air tube syringe needle; Start magnetic agitation, with the heating of big open end glassware, the temperature of controlling solution in the big open end glassware is 45 ~ 55 ℃, begins reaction;
(3) liquid level of solution height in the time recording graduated cylinder, until liquid level is constant, record volume V corresponding to last liquid level 1Calculate hydrogen volume=(V 0-V 1) mL; The burning ash Gold Samples belongs to the quality of aluminium=(V 0-V 1) * 0.8036 * 10 -3g
The burning ash Gold Samples belongs to the mass percentage concentration of aluminium=[(V 0-V 1) * 0.8036 * 10 -3/ M] * 100%.
2. the method for claim 1, is characterized in that described big open end glassware volume V b, the graduated cylinder volume V 0, sodium hydroxide solution volume V NaOHSatisfy following relation:
(1/10)V b≤(V NaOH- V 0)<(V b –V 0)。
3. the method for claim 1, is characterized in that the diameter of described graduated cylinder small hole at bottom part is less than 0.5cm.
4. the method for claim 1, is characterized in that described big open end glassware is large beaker, and described little open glass vessel are small beaker.
5. device that detects metallic aluminium content in burning ash, it is characterized in that described device comprises the big open end glassware, is positioned over the little open glass vessel of the burning ash the placed sample in the big open end glassware, the graduated cylinder of bottom perforate, an end connects the air tube syringe needle of aspiration pump; Be placed with magnetic stirring bar in described little open glass vessel; The graduated cylinder of bottom perforate is inverted, and covers the little open glass vessel in the big open end glassware, the aperture rubber pad hermetic seal of graduated cylinder bottom; Described big open end glassware is positioned on the well heater of temp. controllable, and is provided with thermometer in described big open end glassware, and described well heater has magnetic stirring function.
6. device as claimed in claim 5, is characterized in that described big open end glassware is large beaker, and described little open glass vessel are small beaker.
7. device as claimed in claim 5 is characterized in that the volume V of described big open end glassware bThe volume V of mL and little open glass vessel sThe ratio of mL is 15-100:1.
8. device as claimed in claim 5, the volume that it is characterized in that described graduated cylinder is V 0ML, and V b– V 0>0.
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CN103808629A (en) * 2014-03-07 2014-05-21 周长祥 Phase analysis method for metal zinc in hot-dip galvanized ashes
CN104198329A (en) * 2014-09-05 2014-12-10 天津立中合金集团有限公司 Method and device for rapidly detecting content of metallic aluminum in aluminum ash
WO2016102208A1 (en) * 2014-12-23 2016-06-30 Umicore Composite powder for use in an anode of a lithium ion battery, method of preparing such a composite powder and method for analysing such a composite powder
CN107202865A (en) * 2017-05-12 2017-09-26 上海大学 Heavy metal stabilizing and the quick determination method of toxicity in domestic garbage incineration flyash
CN109507385A (en) * 2018-12-07 2019-03-22 中国工程物理研究院化工材料研究所 A kind of active aluminium content measuring device and its application method

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CN103389256A (en) * 2013-07-18 2013-11-13 烟台大学 Method for measuring metal aluminum content in garbage incineration slag
CN103808629A (en) * 2014-03-07 2014-05-21 周长祥 Phase analysis method for metal zinc in hot-dip galvanized ashes
CN104198329A (en) * 2014-09-05 2014-12-10 天津立中合金集团有限公司 Method and device for rapidly detecting content of metallic aluminum in aluminum ash
WO2016102208A1 (en) * 2014-12-23 2016-06-30 Umicore Composite powder for use in an anode of a lithium ion battery, method of preparing such a composite powder and method for analysing such a composite powder
CN107408676A (en) * 2014-12-23 2017-11-28 尤米科尔公司 The method of composite powder in lithium-ions battery anode, the method for preparing this composite powder and this composite powder of analysis
US20170352877A1 (en) * 2014-12-23 2017-12-07 Umicore Composite Powder for Use in an Anode of a Lithium Ion Battery, Method of Preparing such a Composite Powder and Method for Analysing such a Composite Powder
US10483529B2 (en) * 2014-12-23 2019-11-19 Umicore Composite powder for use in an anode of a lithium ion battery, method of preparing such a composite powder and method for analysing such a composite powder
CN107202865A (en) * 2017-05-12 2017-09-26 上海大学 Heavy metal stabilizing and the quick determination method of toxicity in domestic garbage incineration flyash
CN107202865B (en) * 2017-05-12 2020-08-21 上海大学 Method for rapidly detecting stability and toxicity of heavy metals in household garbage incineration fly ash
CN109507385A (en) * 2018-12-07 2019-03-22 中国工程物理研究院化工材料研究所 A kind of active aluminium content measuring device and its application method

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