CN108479720A - Using mussel shell as the nanometer demercuration design of material and preparation method of raw material - Google Patents
Using mussel shell as the nanometer demercuration design of material and preparation method of raw material Download PDFInfo
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- CN108479720A CN108479720A CN201810386840.4A CN201810386840A CN108479720A CN 108479720 A CN108479720 A CN 108479720A CN 201810386840 A CN201810386840 A CN 201810386840A CN 108479720 A CN108479720 A CN 108479720A
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- mussel shell
- demercuration
- nanometer
- mussel
- design
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells
Abstract
The present invention discloses a kind of using mussel shell as the nanometer demercuration design of material method of raw material, includes the following steps：Collect typical mussel shell；Phenetic analysis is carried out to mussel shell sample, builds mussel shell database；Mussel shell sample is modified processing；According to the mixed proportion of a variety of mussel shell materials, a variety of nanometers of demercuration material prescriptions are formulated；A variety of mussel shell materials are mixed according to the ratio according to formula, a nanometer demercuration material is prepared；The mercury adsorption capacity for testing nanometer demercuration material, evaluates and screens nanometer demercuration material；In-situ characterization is carried out to nanometer demercuration material.Coal-fired Hg control technologies and environmental improvement investigation of materials are combined by the present invention, provide a kind of using mussel shell as the coal-fired flue-gas mercury removal material of raw material, are peomoted coastal solid waste mussel shell comprehensive utilization of resources, are realized the treatment of wastes with processes of wastes against one another, develop a circular economy.
Description
Technical field
The present invention relates to coal-fired flue gas mercury removal field of material technology, and in particular to a kind of de- by the nanometer of raw material of mussel shell
Mercury design of material and preparation method.
Background technology
Coal-burning power plant, coal-burning boiler, oil refining industry, non-ferrous metal metallurgy industry, waste incineration and generating electricity and a huge sum of money
Belong to contaminated land administer and the flue gas exhaust gas of recovery project in and the fossils energy such as coke-stove gas, water-gas, natural gas and shale gas
All contain heavy metal Hg in the correlation combustion gas of source.Mercury is due to hypertoxicity, effumability, persistence and deposition in vivo
Property and become the toxic carcinogenic contaminant of air of greatest concern after sulfur dioxide and nitrogen oxides.Mercury is to organism and environment
Prodigious harm is caused, the mercury discharged from above-mentioned industry can propagate hundreds of kilometer in air, penetrate into each ring of food chain
Section, even if far from mercury pollution source, fish, domestic animal, crops still can be contaminated.And organism can be anti-in vivo after absorbing mercury
The methyl mercury that severe toxicity should be formed, to destroy the analytic metabolism function of biological cell.Afterbody of the mankind as food chain,
Mercury in allogene body can be recycled into human body after enrichment, can cause a series of health problem.On the other hand, with
The fast development of region following the line of the sea mussel culture and processing industry generates a large amount of shells, and discarded mussel shell causes coastal ecological environment
Serious pollution, it has also become coastal area environmental hazard urgently to be resolved hurrily.
In view of drawbacks described above, creator of the present invention obtains the present invention finally by prolonged research and practice.
Invention content
To solve above-mentioned technological deficiency, the technical solution adopted by the present invention is, provides a kind of using mussel shell as raw material
Nanometer demercuration design of material and preparation method, include the following steps：
S100：Typical mussel shell is collected, powdered mussel shell sample is made；
S200：Phenetic analysis is carried out to the mussel shell sample, records the analysis data of the various mussel shell samples, structure
Build mussel shell database；
S300：The mussel shell sample is modified processing, one-component is obtained and is modified mussel shell material；
S400：It is modified the mixed proportion of mussel shell material according to a variety of one-components, formulates a variety of nanometers of demercuration materials
Formula；
S500：A variety of one-components are modified mussel shell material according to the formula to mix according to the ratio, is prepared and receives
Rice demercuration material；
S600：The mercury adsorption capacity for testing the nanometer demercuration material evaluates and screens the nanometer demercuration material；
S700：In-situ characterization is carried out to the nanometer demercuration material.
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 1h, removes surface impurity, is put into high speed disintegrator and crushes, and the sieving of 60-100 mesh obtains powdered mussel shell
Sample.
Preferably, the step S200 is specially：Using mussel shell sample surfaces form described in scanning electron microscopic observation；Using
Than specific surface area, pore volume and the pore-size distribution that table analyzer measures the mussel shell sample；It is analyzed using X-ray fluorescence spectra
Element species and content in the mussel shell sample；The phenetic analysis data of each mussel shell sample are recorded, structure is made a gift of
Shell database.
Preferably, the step S300 is specially：The mussel shell sample is dissolved in excess silicic acid sodium solution, is placed in Muffle
Calcining in stove, is warming up to 200-250 DEG C, reacts 30-60min, filters out solid；The solid of filtering is placed in Muffle furnace and is forged
It burns, calcination temperature is 400-600 DEG C, reaction time 30-120min；Solid after calcining is crushed, is cooled to room temperature, 60-
100 mesh are sieved, and obtain one-component and are modified mussel shell material.
Preferably, utilizing the formula of first-principles calculations simulation demercuration nano material in the step S400.
Preferably, the step S500 is specially：A variety of one-components are modified ratio of the mussel shell material in the formula
Mixing, by mixture in planetary ball mill mix grinding 10-15min；Mixture is heated to 300-500 DEG C in electric furnace, heating
1-3h；Product after heating is taken out, it is washed and is filtered with hot distilled water, obtained sediment drying is received
Rice demercuration material.
Preferably, tested in the step S600 mercury adsorption capacity of the nanometer demercuration material the specific steps are：It takes
1-2g material samples are put into solid-bed reactor；Gaseous state Hg is generated by mercury vapour generator, enters institute by carrier of nitrogen
It states solid-bed reactor, controls gas flow 1-2L/min, a concentration of 30-35ug/m3 of Hg in gas；The Solid Bed reaction
Device is warming up to 800 DEG C since 20 DEG C with the rate of heat addition of 1-5 DEG C/min；It is online that the tail gas of the solid-bed reactor enters mercury
Analysis system, the continuous content for measuring Hg in air-flow.
Preferably, being evaluated and screened to the nanometer demercuration material by high throughput experiment in the step S600.
Preferably, the step S700 is specially：Infrared spectrum analysis is carried out to the nanometer demercuration material, and builds and receives
The characteristic infrared spectrum library of rice demercuration material.
Compared with the prior art the beneficial effects of the present invention are：
Coal-fired Hg control technologies and environmental improvement investigation of materials are combined by the present invention, and it is original to provide one kind with mussel shell
The coal-fired flue-gas mercury removal material of material peomotes coastal solid waste mussel shell comprehensive utilization of resources, realizes the treatment of wastes with processes of wastes against one another,
It develops a circular economy.Invention has expanded material genetic engineering in the new of the field of environmental improvement such as solid waste improvement and Air Pollution Control
Using, and corresponding material gene pool is constructed, there is great environment, economic and social benefit.
Description of the drawings
It is required in being described below to embodiment 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 using mussel shell as the flow chart of the nanometer demercuration design of material and preparation method of raw material；
Fig. 2 is the flow chart of mussel shell characterizing method；
Fig. 3 is the flow chart of mussel shell modification processing method；
Fig. 4 is to prepare a nanometer flow chart for demercuration MATERIALS METHODS；
Fig. 5 is a nanometer flow chart for demercuration material mercury adsorption capacity test method.
Specific implementation mode
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 demercuration performance.The present invention proposes a kind of receiving using mussel shell as raw material
Rice demercuration design of material and preparation method, as shown in Figure 1, including the following steps：
S100：Typical mussel shell is collected, mussel shell is cleaned with clear water, 1h is impregnated with dilute hydrochloric acid, removes surface impurity,
It is put into high speed disintegrator and crushes, the sieving of 60-100 mesh obtains powdered mussel shell sample.
S200：Phenetic analysis is carried out to a variety of mussel shell samples, records the analysis data of the various mussel shell samples, structure
Build mussel shell database.Mussel shell type includes emerald shell, Mytilus galloprovincialis shell, thick shell etc., the mussel shell root in each type
Can also have different physicochemical characteristics according to factors such as growing environment, aquaculture sea area, growth times, it is therefore desirable to different mussels
Shell carries out phenetic analysis to build complete database.
As shown in Fig. 2, the characterization of mussel shell includes the following steps：
S210：Using scanning electron microscopic observation mussel shell sample surfaces form.
S220：Using specific surface area, pore volume and the pore-size distribution for measuring mussel shell sample than table analyzer.
S230：Element species and content in mussel shell sample are analyzed using X-ray fluorescence spectra.
S300：Mussel shell is modified processing, obtains the modification mussel shell nanometer demercuration material of one-component.Such as Fig. 3 institutes
Show, the modification of mussel shell includes the following steps：
S310：Powdered mussel shell sample is dissolved in excessive sodium silicate solution, calcines, is warming up in merging Muffle furnace
200-250 DEG C, 30-60min is reacted, solid is filtered out.
S320：The solid of filtering is placed in Muffle furnace and is calcined, is calcined as temperature at 400-600 DEG C, time 30-
120min。
S330：Solid is crushed, is cooled to room temperature, the sieving of 60-100 mesh obtains one-component and is modified mussel shell material.
S400：It is modified the mixed proportion of mussel shell material according to a variety of one-components, formulates a variety of nanometers of demercuration materials
Formula.The present embodiment can be designed using the formula of first-principles calculations simulation demercuration nano material with high adsorption energy
The demercuration nano material formula of power improves working efficiency.
S500：A variety of one-components are modified mussel shell material according to the formula of design to mix according to the ratio, are prepared
Nanometer demercuration material.As shown in figure 4, specifically including following steps：
S510：A variety of one-components are modified ratio mixing of the mussel shell material by the formula, mixture is expert at celestial body
Mix grinding 10-15min in grinding machine.
S520：Mixture is heated to 300-500 DEG C in electric furnace, heats 1-3h；
S530：Product after heating is taken out, it is washed and is filtered with hot distilled water, obtained sediment is through drying
It is dry to obtain a nanometer demercuration material.
The preparation method operating condition is mild, simple for process, equipment investment and energy consumption, is suitable for industrial mass production.
S600：The mercury adsorption capacity for testing the nanometer demercuration material, by high throughput experiment to the nanometer demercuration material
Material is evaluated and screened.As shown in figure 5, the specific testing procedure of the mercury adsorption capacity of nanometer demercuration material is：
S610：1-2g material samples are taken to be put into solid-bed reactor；
S620：Gaseous state Hg is generated by mercury vapour generator, enters solid-bed reactor by carrier of nitrogen, controls gas
Flow 1-2L/min, a concentration of 30-35ug/m3 of Hg in gas；
S630：Solid-bed reactor is warming up to 800 DEG C since 20 DEG C with the rate of heat addition of 1-5 DEG C/min；
S640：The tail gas of solid-bed reactor enters mercury on-line analysis system, and the continuous content for measuring Hg in air-flow passes through
This method can quickly measure a nanometer adsorption capacity for demercuration material.
S700：In-situ characterization is carried out to nanometer demercuration material, infrared spectrum analysis is carried out to nanometer demercuration material, and build
Characteristic infrared spectrum library can tentatively judge the mercury adsorption capacity of mussel shell material according to infrared spectrum later.
Coal-fired Hg control technologies and environmental improvement investigation of materials are combined by the present invention, provide a kind of new coal-fired flue-gas
Mercury removal material peomotes coastal solid waste mussel shell comprehensive utilization of resources, realizes the treatment of wastes with processes of wastes against one another, development cycle warp
Ji.Data analysis is carried out additionally by mussel shell database, high-throughput experimental data and characteristic infrared spectrum library, can be built
Complete set using mussel shell as the nanometer demercuration material prescription system of raw material, have good application prospect.
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 changes or even equivalent, but falls in protection scope of the present invention.
Claims (9)
1. a kind of using mussel shell as the nanometer demercuration design of material and preparation method of raw material, which is characterized in that include the following steps：
S100：Typical mussel shell is collected, powdered mussel shell sample is made；
S200：Phenetic analysis is carried out to the mussel shell sample, records the analysis data of the various mussel shell samples, structure is made a gift of
Shell database；
S300：The mussel shell sample is modified processing, one-component is obtained and is modified mussel shell material；
S400：It is modified the mixed proportion of mussel shell material according to a variety of one-components, formulates a variety of nanometers of demercuration material prescriptions；
S500：A variety of one-components are modified mussel shell material according to the formula to mix according to the ratio, it is de- that nanometer is prepared
Mercury material；
S600：The mercury adsorption capacity for testing the nanometer demercuration material evaluates and screens the nanometer demercuration material；
S700：In-situ characterization is carried out to the nanometer demercuration material.
2. as described in claim 1 using mussel shell as the nanometer demercuration design of material and preparation method of raw material, which is characterized in that
The step S100 is specially：Typical mussel shell is collected, the mussel shell is cleaned with clear water, 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. as claimed in claim 2 using mussel shell as the nanometer demercuration design of material and preparation method of raw material, which is characterized in that
The step S200 is specially：
Using mussel shell sample surfaces form described in scanning electron microscopic observation；
Using specific surface area, pore volume and the pore-size distribution for measuring the mussel shell sample than table analyzer；
Element species and content in the mussel shell sample are analyzed using X-ray fluorescence spectra；
The phenetic analysis data of each mussel shell sample are recorded, mussel shell database is built.
4. as claimed in claim 2 using mussel shell as the nanometer demercuration design of material and preparation method of raw material, which is characterized in that
The step S300 is specially：
The mussel shell sample is dissolved in excess silicic acid sodium solution, is calcined in merging Muffle furnace, is warming up to 200-250 DEG C, reaction
30-60min filters out solid；
The solid of filtering is placed in Muffle furnace and is calcined, calcination temperature is 400-600 DEG C, reaction time 30-120min；
Solid after calcining is crushed, is cooled to room temperature, the sieving of 60-100 mesh obtains one-component and is modified mussel shell material.
5. as claimed in claim 4 using mussel shell as the nanometer demercuration design of material and preparation method of raw material, which is characterized in that
The step S500 is specially：
A variety of one-components are modified mussel shell material to mix in the ratio of the formula, by mixture in planetary ball mill
Mix grinding 10-15min；
Mixture is heated to 300-500 DEG C in electric furnace, heats 1-3h；
Product after heating is taken out, it is washed and is filtered with hot distilled water, sediment is dried, obtains a nanometer demercuration
Material.
6. as described in claim 1 using mussel shell as the nanometer demercuration design of material and preparation method of raw material, which is characterized in that
Tested in the step S600 mercury adsorption capacity of the nanometer demercuration material the specific steps are：
Nanometer demercuration material sample described in 1-2g is taken to be put into solid-bed reactor；
Gaseous state Hg is generated by mercury vapour generator, enters the solid-bed reactor by carrier of nitrogen, controls gas flow
1-2L/min, a concentration of 30-35ug/m3 of Hg in gas；
The solid-bed reactor is warming up to 800 DEG C since 20 DEG C with the rate of heat addition of 1-5 DEG C/min；
The tail gas of the solid-bed reactor enters mercury on-line analysis system, the continuous content for measuring Hg in air-flow.
7. as described in claim 1 using mussel shell as the nanometer demercuration design of material and preparation method of raw material, which is characterized in that
The formula of first-principles calculations simulation demercuration nano material is utilized in the step S400.
8. as claimed in claim 7 using mussel shell as the nanometer demercuration design of material and preparation method of raw material, which is characterized in that
The nanometer demercuration material is evaluated and screened by high throughput experiment in the step S600.
9. as claimed in claim 8 using mussel shell as the nanometer demercuration design of material and preparation method of raw material, which is characterized in that
The step S700 is specially：Infrared spectrum analysis, and construction feature infared spectrum library are carried out to the nanometer demercuration material.
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| CN201810386840.4A CN108479720A (en) | 2018-04-26 | 2018-04-26 | Using mussel shell as the nanometer demercuration design of material and preparation method of raw material |
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| CN201810386840.4A CN108479720A (en) | 2018-04-26 | 2018-04-26 | Using mussel shell as the nanometer demercuration design of material and preparation method of raw material |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101690882A (en) * | 2009-10-14 | 2010-04-07 | 南开大学 | Natural adsorbent for removing heavy metal ions in water and preparation method and application thereof |
| CN104877808A (en) * | 2015-06-26 | 2015-09-02 | 浙江海洋学院 | Method for preparing aquatic product cleaning agent based on shell powder |
| CN105779171A (en) * | 2016-04-07 | 2016-07-20 | 中海得金科技有限公司 | Micro-nano shell powder fruit-vegetable cleaning agent and preparation method thereof |
| WO2016184518A1 (en) * | 2015-05-20 | 2016-11-24 | S.A. Lhoist Recherche Et Developpement | Lime-based sorbent composition for mercury removal and its manufacturing process |
-
2018
- 2018-04-26 CN CN201810386840.4A patent/CN108479720A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101690882A (en) * | 2009-10-14 | 2010-04-07 | 南开大学 | Natural adsorbent for removing heavy metal ions in water and preparation method and application thereof |
| WO2016184518A1 (en) * | 2015-05-20 | 2016-11-24 | S.A. Lhoist Recherche Et Developpement | Lime-based sorbent composition for mercury removal and its manufacturing process |
| CN104877808A (en) * | 2015-06-26 | 2015-09-02 | 浙江海洋学院 | Method for preparing aquatic product cleaning agent based on shell powder |
| CN105779171A (en) * | 2016-04-07 | 2016-07-20 | 中海得金科技有限公司 | Micro-nano shell powder fruit-vegetable cleaning agent and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| SUSANA PEÑA-RODRÍGUEZ ET AL.: "Mercury removal using ground and calcined mussel shell", 《JOURNAL OF ENVIRONMENTAL SCIENCES》 * |
| 师琦 等: "沉淀法SiO2包覆纳米CaCO3吸附剂性能", 《化工学报》 * |
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