CN108828141A - A kind of heavy metal adsorption performance test methods of mussel shell material - Google Patents
A kind of heavy metal adsorption performance test methods of mussel shell material Download PDFInfo
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- CN108828141A CN108828141A CN201810385795.0A CN201810385795A CN108828141A CN 108828141 A CN108828141 A CN 108828141A CN 201810385795 A CN201810385795 A CN 201810385795A CN 108828141 A CN108828141 A CN 108828141A
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
- G01N21/6404—Atomic fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
- G01N2021/3107—Cold vapor, e.g. determination of Hg
Abstract
The present invention discloses a kind of heavy metal adsorption performance test methods of mussel shell material, includes the following steps：S100：A variety of mussel shells are collected, powdered mussel shell sample is made；S200：The mussel shell sample is characterized；S300：Classified according to characterize data to mussel shell；S400：It takes mussel shell sample described in every class to be modified, the modified mussel shell material of multiclass is made；S500：Measure the heavy metal adsorption of modified mussel shell material described in every class.The present invention provides a kind of mussel shell material property integrated test facilities, mussel shell physical and chemical performance can quickly be measured using this method, complete evaluation of material, data are provided as the application of adsorbent for mussel shell material to support, mussel shell material effective classification has been subjected to, and corresponding material database is constructed, there is great environment and economic benefit.
Description
Technical field
The present invention relates to nano adsorption material fields, and in particular to a kind of heavy metal adsorption performance of mussel shell material
Test method.
Background technique
In recent years, with the fast development of region following the line of the sea mussel culture and processing industry, a large amount of shells are produced, discard mussel shell
Serious pollution is caused to coastal ecological environment, it has also become coastal area environmental hazard urgently to be resolved.And pass through the study found that
Mussel shell is a kind of natural poromerics, has potential absorption property.At the same time, the problem of environmental pollution of coal-fired flue-gas
Also it is increasingly subject to people's attention, the discharge for administering pollutant in coal-fired flue-gas has become and need currently solve the problems, such as.In order to incite somebody to action
Discarded mussel shell carries out efficient resource utilization, considers using useless mussel shell as the adsorbent for administering coal-fired flue-gas, but mussel shell is made
For natural material, there is very big difference in the heavy metal adsorption between each mussel shell, in the prior art without one kind
Effective mussel shell material performance test method, can not establish the mussel shell database of system, become mussel shell material apply and
The significant obstacle of research field.
In view of the above drawbacks, creator of the present invention obtains the present invention by prolonged research and practice finally.
Summary of the invention
To solve above-mentioned technological deficiency, the technical solution adopted by the present invention is, provides a huge sum of money for a kind of mussel shell material
Belong to adsorption capacity performance test methods, includes the following steps：
S100：A variety of mussel shells are collected, powdered mussel shell sample is made；
S200：The mussel shell sample is characterized；
S300：Classified according to characterize data to mussel shell；
S400：It takes mussel shell sample described in every class to be modified, the modified mussel shell material of multiclass is made；
S500：Measure the heavy metal adsorption of modified mussel shell material described in every class.
Preferably, the step S100 is specially：Typical mussel shell is collected, the mussel shell is cleaned with clear water, is used
Dilute hydrochloric acid impregnates 0.5-1h, removes surface impurity, is put into high speed disintegrator and crushes, and the sieving of 60-100 mesh obtains powdered make a gift of
Shell sample.
Preferably, including one or more of to the mussel shell sample characterization content in the step S200：Scanning
Electronic Speculum, X-ray diffraction spectra analysis, specific surface opening size test and coal ash meltbility detection.
Preferably, the step S300 is specially：
S310：Intersect the characterize data for comparing every kind of mussel shell sample, obtains between every kind of mussel shell sample
Similarity；
S320：Similar threshold value is set, the similarity between the mussel shell sample and the similar threshold value, when two kinds
When the similarity of the mussel shell sample is higher than the similar threshold value, two kinds of mussel shells are attributed to similar；
S330：The similar mussel shell sample is combined, the classification of mussel shell is completed.
Preferably, the step S310 is specially：The mussel shell sample intersect two-by-two and is compared, and compares two samples
Between every kind of characterize data similarity, set each characterize data weight, the similarity of each characterize data asked by weight
With obtain the similarity between the mussel shell sample.
Preferably, the step S400 is specially：
S410：The mussel shell sample is dissolved in excess silicic acid sodium solution, calcining in merging Muffle furnace is warming up to 200-
250 DEG C, 30-60min is reacted, solid is filtered out；
S420：The solid of filtering is placed in Muffle furnace and is calcined, calcination temperature is 400-600 DEG C, reaction time 30-
120min；
S430：Calcined solid is crushed, is cooled to room temperature, the sieving of 60-100 mesh obtains modified mussel shell material.
Preferably, the step S500 is specially：
S510：Coal sample 20g is taken, is ground to 100-300 microns, the coal sample is placed in reactor, is added described in 1-2g
Modified mussel shell material；
S520：Nitrogen purge air is passed through into the reactor, the reactor is added from room temperature with 10-15 DEG C/min
Heat is to 700-900 DEG C, after reaching reaction temperature, constant temperature 5-15min；
S530：Closing air inlet and heating power supply makes whole system natural cooling, collects gasification product, measures the gasification and produces
Content of beary metal in object.
Preferably, the metallic element for measuring the gasification product in the step S530 includes arsenic, chromium, cadmium, lead and mercury.
Preferably, the method also includes step S600：Record the characterize data and heavy metal adsorption energy of every class mussel shell
Force data constructs mussel shell material database.
Compared with the prior art the beneficial effects of the present invention are：
The present invention provides a kind of efficient mussel shell material all-round property testing methods, can be to mussel using this method
Shell physical and chemical performance is quickly measured, and evaluation of material is completed, and the application for mussel shell material as adsorbent provides data branch
It holds, peomotes coastal solid waste mussel shell comprehensive utilization of resources, realize waste treatment and waste, develop a circular economy.Invention is logical
Similarity comparison is crossed, mussel shell material has been subjected to effective classification, and construct corresponding material database, there is great ring
Border and economic benefit.
Detailed description of the invention
It, below will be to required in embodiment description in order to illustrate more clearly of the technical solution in various embodiments of the present invention
The attached drawing used is briefly described.
Fig. 1 is the flow chart of the heavy metal adsorption performance test methods of mussel shell material；
Fig. 2 is the flow chart for carrying out classification method to mussel shell according to characterize data；
Fig. 3 is the flow chart for preparing modified mussel shell MATERIALS METHODS；
Fig. 4 is the flow chart of heavy metal adsorption measuring method.
Specific embodiment
Below in conjunction with attached drawing, the forgoing and additional technical features and advantages are described in more detail.
Mussel shell is a kind of natural micropore mineralizing material, and main chemical analysis includes Ca and microchemistry ingredient
Cu, Zn, Fe, Co, Ni, Mn, Mg etc., with potential absorption property.The present invention provides a kind of heavy metal of mussel shell material
Adsorption capacity performance test methods can quickly measure mussel shell physical and chemical performance, complete evaluation of material, be mussel shell material
Expect that the application as adsorbent provides data and supports.As shown in Fig. 1, this approach includes the following steps：
S100：A variety of typical mussel shells are collected, mussel shell is cleaned with clear water, 1h is impregnated with dilute hydrochloric acid, removes surface
Impurity is put into high speed disintegrator and crushes, and the sieving of 60-100 mesh obtains powdered mussel shell sample, powdered mussel shell sample
Conducive to subsequent performance test.
S200：Each mussel shell sample is characterized, characterization content includes scanning electron microscope, X-ray diffraction spectra point
Analysis, specific surface opening size test and coal ash meltbility detection.
Wherein scanning electron microscope analysis step is：By mussel shell sample uniformly smear in the nail pattern sample platform for posting carbon ribbon
On, it is ensured that sample fills carbon ribbon uniformly to reduce the influence to element measurement, and above-mentioned sample stage is put into scanning electron microscope observation ash
Sample configuration of surface simultaneously measure sample element composition, carry out EDX test when, acceleration voltage to be generally arranged in 10-20keV it
Between with ensure EDX probe can be collected into enough x-rays, obtain mussel shell sample surfaces form.
X-ray diffraction spectra analytical procedure is：50kV is set by x-ray tube voltage, electric current 1mA uses X-ray tube
The x-ray generated excites sample to be tested, will radiate different secondary x rays and different intensity according to different elements
To measure element species and content in sample.
Specific surface and opening size test step are：The specific surface area and void determination instrument used, based on draw opposite pressure and
The variation relation of the multi-molecular absorption of nitrogen obtains the specific surface area of mussel shell sample, while instrument can be de- by adsorbing
Attached automated image analysis pore volume and pore size.
Coal ash meltbility detecting step is：Mussel shell sample is put into coal ash meltbility detector, heating obtains sample
Coal ash meltbility curve.
Mussel shell sample side is characterized, can be selected in above-mentioned characterizing method, carry out one or more characterizations.Knot
A variety of characterization methods are closed, it being capable of comprehensive physicochemical characteristic that must detect mussel shell sample.
S300：Classified according to characterize data to mussel shell, as shown in Fig. 2, classification method includes the following steps：
S310：Mussel shell sample intersect two-by-two and is compared, and compares the similarity of every kind of characterize data between two samples.
Wherein scanning electron microscope analysis passes through image alignment similarity；X-ray diffraction spectra analysis is similar by constituent content contrast conting
Degree；Specific surface opening size test passes through specific surface area and aperture contrast conting similarity；Coal ash meltbility detection is special by ash melting
Linearity curve is fitted alignment similarity, and the above similarity comparison result is acquired by computer program.
Each characterize data weight is set, the similarity of each characterize data is summed by weight, obtains the mussel shell
Similarity between sample.Calculating formula of similarity i.e. between mussel shell sample is：
Fi=Tα+Cβ+Kγ+Qδ；
Wherein similarity of the Fi between mussel shell sample, T are scanning electron microscope image similarity, and α is scanning electron microscope image
Similarity weight, C are constituent content similarity, and β is constituent content similarity weight, and K is specific surface area similarity, and γ is than table
Area similarity weight, Q are coal ash meltbility curve similarity, and δ is coal ash meltbility curve similarity weight.
S320：Similar threshold θ is set, compares similarity and similar threshold value between mussel shell sample, when two kinds of mussel shells
The corresponding two kinds of mussel shells of both mussel shell samples are attributed to similar by the high Fi > θ of the similarity of sample；
S330：Similar mussel shell sample is combined and is summarized, the classification of mussel shell is completed.
Due to mussel shell wide variety, the materialization of every kind of mussel shell characterizes difference, there is the performance of mussel shell material very
Big difference, the similarity comparison of passage capacity of the present invention are effectively classified mussel shell material, can be used as mussel shell data
The basis that library is established, is conducive to the comprehensive study and utilization of mussel shell.
S400：It takes mussel shell sample described in every class to be modified, the modified mussel shell material of multiclass is made.As shown in Fig. 3,
The modification of mussel shell material includes step in detail below：
S410：Mussel shell sample is dissolved in excess silicic acid sodium solution, calcining in merging Muffle furnace is warming up to 200- 250
DEG C, 30-60min is reacted, solid is filtered out；
S420：The solid of filtering is placed in Muffle furnace and is calcined, calcination temperature is 400-600 DEG C, reaction time 30-
120min；
S430：Calcined solid is crushed, is cooled to room temperature, the sieving of 60-100 mesh obtains modified mussel shell material.
S500：The heavy metal adsorption of the modified mussel shell material of every class is measured, it is right because mussel shell has absorption potential
The modification mussel shell material of classification carries out absorption property test, and the application for mussel shell material as adsorbent provides data branch
It holds, peomotes coastal solid waste mussel shell comprehensive utilization of resources, realize waste treatment and waste.As shown in figure 4, being inhaled to heavy metal
Attached ability determination step is：
S510：Coal sample 20g is taken, is ground to 100-300 microns, the coal sample is placed in reactor, it is modified that 1-2g is added
Mussel shell material；
S520：Nitrogen purge air is passed through into reactor, the reactor is heated from room temperature, and the rate of heat addition is in 10-15
DEG C/min between select, outlet temperature selects between 700-900 DEG C, after temperature of reaching home, constant temperature for a period of time, constant temperature
Time selects between 5-15min；
S530：Closing air inlet and heating power supply makes whole system natural cooling, collects gasification product, measures in gasification product
Content of beary metal.The heavy metal element contained in coal-fired flue-gas includes arsenic, chromium, cadmium, lead and mercury, is needed to these heavy metal elements
Content is tested respectively, to measure modified mussel shell material to the absorption property of different heavy metal elements.Atom can be used
The content of fluorescence spectrometry element arsenic uses cold-vapour atomic absorption method using the content of aas determination elemental chromium, cadmium and lead
Measure the content of element mercury.
This method tests the vertical distribution content generated in coal gasifying process, has rated every class mussel shell
Material can be used as the data foundation for formulating mixing mussel shell adsorbent material formula to the adsorption capacity of each metallic element.
S600：The characterize data and heavy metal adsorption data of every class mussel shell are recorded, mussel shell material data is constructed
Library.The materialization characterization and adsorption capacity of mussel shell material are recorded according to classification, complete mussel shell material can be constructed
Gene database, the basis that mussel shell material database is researched and developed as mussel shell new material have great environment and economy
Benefit.
The foregoing is merely presently preferred embodiments of the present invention, is merely illustrative for the purpose of the present invention, and not restrictive
's.Those skilled in the art understand that in the spirit and scope defined by the claims in the present invention many changes can be carried out to it,
It modifies or even equivalent, but falls in protection scope of the present invention.
Claims (9)
1. a kind of heavy metal adsorption performance test methods of mussel shell material, which is characterized in that include the following steps：
S100：A variety of mussel shells are collected, powdered mussel shell sample is made；
S200：The mussel shell sample is characterized；
S300：Classified according to characterize data to mussel shell；
S400：It takes mussel shell sample described in every class to be modified, the modified mussel shell material of multiclass is made；
S500：Measure the heavy metal adsorption of modified mussel shell material described in every class.
2. the heavy metal adsorption performance test methods of mussel shell material as described in claim 1, which is characterized in that described
Step S100 is specially：Typical mussel shell is collected, the mussel shell is cleaned with clear water, 0.5-1h is impregnated with dilute hydrochloric acid, removes
Surface impurity is removed, is put into high speed disintegrator and crushes, the sieving of 60-100 mesh obtains powdered mussel shell sample.
3. the heavy metal adsorption performance test methods of mussel shell material as claimed in claim 2, which is characterized in that described
It include one or more of to the mussel shell sample characterization content in step S200：Scanning electron microscope, X-ray diffraction spectra point
Analysis, specific surface opening size test and coal ash meltbility detection.
4. the heavy metal adsorption performance test methods of mussel shell material as described in claim 1, which is characterized in that described
Step S300 is specially：
S310：Intersect the characterize data for comparing every kind of mussel shell sample, obtains the phase between every kind of mussel shell sample
Like degree；
S320：Similar threshold value is set, the similarity between the mussel shell sample and the similar threshold value, described in two kinds
When the similarity of mussel shell sample is higher than the similar threshold value, both mussel shells are attributed to similar；
S330：Similar mussel shell is combined and is summarized, the classification of mussel shell is completed.
5. the heavy metal adsorption performance test methods of mussel shell material as claimed in claim 4, which is characterized in that described
Step S310 is specially：The mussel shell sample intersect two-by-two and is compared, and compares between two mussel shell samples every kind
The similarity of characterize data sets each characterize data weight, the similarity of each characterize data is asked by weight
With obtain the similarity between the mussel shell sample.
6. the heavy metal adsorption performance test methods of mussel shell material as claimed in claim 2, which is characterized in that described
Step S400 is specially：
S410：The mussel shell sample is dissolved in excess silicic acid sodium solution, calcining in merging Muffle furnace is warming up to 200-250 DEG C,
30-60min is reacted, solid is filtered out；
S420：The solid of filtering is placed in Muffle furnace and is calcined, calcination temperature is 400-600 DEG C, reaction time 30-
120min；
S430：Calcined solid is crushed, is cooled to room temperature, the sieving of 60-100 mesh obtains modified mussel shell material.
7. the heavy metal adsorption performance test methods of mussel shell material as claimed in claim 6, which is characterized in that described
Step S500 is specially：
S510：Coal sample 20g is taken, is ground to 100-300 microns, the coal sample is placed in reactor, is added modified described in 1-2g
Mussel shell material；
S520：Nitrogen purge air is passed through into the reactor, the reactor is heated to from room temperature with 10-15 DEG C/min
700-900 DEG C, after reaching reaction temperature, constant temperature 5-15min；
S530：Closing air inlet and heating power supply makes whole system natural cooling, collects gasification product, measures in the gasification product
Content of beary metal.
8. the heavy metal adsorption performance test methods of mussel shell material as claimed in claim 7, which is characterized in that described
The metallic element that the gasification product is measured in step S530 includes arsenic, chromium, cadmium, lead and mercury.
9. the heavy metal adsorption performance test methods of mussel shell material a method as claimed in any one of claims 1-8, feature exist
In the method also includes step S600：The characterize data and heavy metal adsorption data, building for recording every class mussel shell are made a gift of
Shellfish material database.
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Cited By (1)
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| CN113231039A (en) * | 2021-04-16 | 2021-08-10 | 广东产品质量监督检验研究院（国家质量技术监督局广州电气安全检验所、广东省试验认证研究院、华安实验室） | Environment-friendly degradable mercury adsorption bag |
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