CN106493384A - A kind of high-purity Zero-valent Iron biological carbon preparation method - Google Patents

A kind of high-purity Zero-valent Iron biological carbon preparation method Download PDF

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Publication number
CN106493384A
CN106493384A CN201610906553.2A CN201610906553A CN106493384A CN 106493384 A CN106493384 A CN 106493384A CN 201610906553 A CN201610906553 A CN 201610906553A CN 106493384 A CN106493384 A CN 106493384A
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biological carbon
heated
heating rate
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林强
于长江
史载锋
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Hainan Normal University
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Hainan Normal University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/06Ferric oxide [Fe2O3]
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/133Renewable energy sources, e.g. sunlight

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Cosmetics (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

A kind of high-purity Zero-valent Iron biological carbon preparation method of the present invention.Preparation process:(1) 100~200 mesh sieve are crossed after cocoanut husk, Cocos nucifera L. petiole, palm petiole being exposed to the sun, dried, being crushed;(2) iron chloride, ferric nitrate or 20~40g of iron sulfate are taken to be dissolved in dehydrated alcohol, is added, after 20~30h of stirring, stand 20~40 days;(3) step (2) mixed solution supernatant liquid is poured out, after revolving reclaims most of ethanol, solution refunds 3~10h of stirring, after standing 2~3 days, dries to viscous pasty state under conditions of 100 DEG C;(4) mixture of viscous form in step (3) is added in tube furnace; 200 DEG C are heated to the heating rate of 3~5 DEG C/min under conditions of nitrogen or helium protection after 5~15min of evacuation, 5~15min of logical nitrogen or helium; 800 DEG C are heated to afterwards with the heating rate of 10~15 DEG C/min; room temperature is cooled to after keeping 3~4h, high-purity Zero-valent Iron biological carbon is obtained.Effect:Method is simply effective, economical and practical, environmental protection.

Description

A kind of high-purity Zero-valent Iron biological carbon preparation method
Technical field
The invention belongs to chemical field, and in particular to a kind of high-purity Zero-valent Iron biological carbon preparation method.
Background technology
Zero-valent Iron biological carbon generally with liquid-phase chemistry deposition technique prepare, i.e., by iron salt (ferric chloride or ferrous sulfate) with Biological carbon surface loaded to and the Zero-valent Iron that reduction reaction generates in boron hydrogen salt (sodium borohydride or potassium borohydride) there is, but this side There is limitations and shortcoming in method, such as preparation cost is high, and using for boron hydrogen salt may generation environment pollution problem.
Content of the invention
It is an object of the invention to provide a kind of high-purity Zero-valent Iron biological carbon preparation method.
The present invention for the solution technical scheme that adopts of its technical problem is:
A kind of high-purity Zero-valent Iron biological carbon preparation method, it is characterised in that step is as follows:
(1) 100~200 mesh sieve are crossed after first cocoanut husk, Cocos nucifera L. petiole, palm petiole being exposed to the sun, dried, being crushed Make powder;
(2) iron chloride, ferric nitrate or 20~40g of iron sulfate are taken to be dissolved in dehydrated alcohol, is added ~18g, stands 20~40 days after 20~30h of stirring;
(3) step (2) mixed solution supernatant liquid is poured out, after revolving reclaims most of ethanol, solution refunds 3~10h of stirring, After standing 2~3 days, dry to viscous pasty state under conditions of 100 DEG C;
(4) mixture of viscous form in step (3) is added in tube furnace, 5~15min of evacuation, logical nitrogen or helium 5~ 200 DEG C are heated to the heating rate of 3~5 DEG C/min under conditions of nitrogen or helium protection after 15min, afterwards with 10~15 DEG C/heating rate of min is heated to 800 DEG C, room temperature is cooled to after keeping 3~4h, high-purity Zero-valent Iron biological carbon is obtained.
Further, described a kind of high-purity Zero-valent Iron biological carbon preparation method, it is characterised in that:
(1) cross 200 mesh sieve to make after first cocoanut husk, Cocos nucifera L. petiole, palm petiole being exposed to the sun, dried, being crushed Powder;
(2) iron chloride, ferric nitrate or iron sulfate 30g are taken to be dissolved in dehydrated alcohol, is added in step (1) and is obtained powder 12g, stir 30 days are stood after mixing 24h;
(3) step (2) mixed solution supernatant liquid is poured out, after revolving reclaims most of ethanol, solution refunds stirring 5h, stands After 2 days, dry to viscous pasty state under conditions of 100 DEG C;
(4) mixture of viscous form in step (3) is added in tube furnace, in nitrogen after evacuation 10min, logical nitrogen 10min 200 DEG C are heated to the heating rate of 5 DEG C/min under conditions of protection, 800 are heated to the heating rate of 10 DEG C/min afterwards DEG C, room temperature is cooled to after keeping 3h, high-purity Zero-valent Iron biological carbon is obtained.
Further, described high-purity Zero-valent Iron biological carbon preparation method, it is characterised in that:Preparing biological carbon process Middle sharp reduction with carbon ferric ion.
The invention has the beneficial effects as follows:The method of present invention report different from the past, specifically in the mistake for preparing biological carbon In journey, sharp one step of reduction with carbon ferric iron prepares highly purified Zero-valent Iron biological carbon, and preparation method is simple and practical, be a kind of economy, Environmental protection, the new method being more value in use.
Description of the drawings
Fig. 1 is the XRD schematic diagrams that embodiment 1 prepares product;
Fig. 2 is the XRD schematic diagrams that embodiment 2 prepares product;
Fig. 3 is the XRD schematic diagrams that embodiment 3 prepares product;
Fig. 4 is the XRD schematic diagrams that embodiment 4 prepares product;
Fig. 5 is the XRD schematic diagrams that embodiment 5 prepares product;
Fig. 6 is the XRD schematic diagrams that embodiment 6 prepares product;
Fig. 7 is the XRD schematic diagrams that embodiment 7 prepares product.
In figure:● Fe is represented, * represents γ-Fe2O3, represents Fe3O4, ◆ represent Fe3C.
Specific embodiment
A kind of high-purity Zero-valent Iron biological carbon preparation method:
Cocoanut husk is exposed to the sun, dried by this experiment case study first, crush after cross 200 mesh sieve, take iron chloride(FeCl3·6H2O) 30g is dissolved in dehydrated alcohol, is added 200 mesh cocoanut husk powder 12g, is stood 30 days after stirring 24h.By cocoanut husk powder chlorination Ferrum alcohol mixed solution supernatant liquid is poured out, and after revolving reclaims big portion's ethanol, solution refunds stirring 5h, at 100 DEG C after standing 2 days Under conditions of dry to viscous pasty state.The early stage of experiment case study 1-6,8,9 is processed in this way.
Cracking adopts Hefei Ke Jing Materials Technology Ltd. tube furnace, model OTF-1200X-100.Operating process is: Main power source is opened, switch is opened, heating schedule is set, the cocoanut husk powder iron chloride viscous mixture that handles well is added to stone English crucible is put in tube furnace boiler tube, installs plug mouth, and evacuation is cracked after leading to nitrogen under conditions of nitrogen protection, nitrogen Flow velocity is 150mL/min, and after tube furnace is cooled to room temperature, product takes out loading hermetic bag.
Embodiment 1:
Cocoanut husk powder iron chloride viscous mixture is added to silica crucible to be put in tube furnace boiler tube, evacuation 10min, logical 200 DEG C are heated to the heating rate of 5 DEG C/min under conditions of nitrogen protection after nitrogen 10min, afterwards with 10 DEG C/min's Heating rate is heated to 700 DEG C, is cooled to room temperature after keeping 1h.
The product obtained by the present embodiment is γ-Fe2O3Biological carbon.
Embodiment 2:
Cocoanut husk powder iron chloride viscous mixture is added to silica crucible to be put in tube furnace boiler tube, evacuation 10min, logical 200 DEG C are heated to the heating rate of 5 DEG C/min under conditions of nitrogen protection after nitrogen 10min, afterwards with 10 DEG C/min's Heating rate is heated to 700 DEG C, is cooled to room temperature after keeping 3h.
The product obtained by the present embodiment is Fe-FeO-Fe3O4Biological carbon, Fe3+Fe, FeO are mainly reduced into.
Embodiment 3:
Cocoanut husk powder iron chloride viscous mixture is added to silica crucible to be put in tube furnace boiler tube, evacuation 10min, logical 200 DEG C are heated to the heating rate of 5 DEG C/min under conditions of nitrogen protection after nitrogen 10min, afterwards with 10 DEG C/min's Heating rate is heated to 800 DEG C, is cooled to room temperature after keeping 1h.
The product obtained by the present embodiment is Fe-Fe3O4Biological carbon, Fe3+Fe is mainly reduced into.
Embodiment 4:
Cocoanut husk powder iron chloride viscous mixture is added to silica crucible to be put in tube furnace boiler tube, evacuation 10min, logical 200 DEG C are heated to the heating rate of 5 DEG C/min under conditions of nitrogen protection after nitrogen 10min, afterwards with 10 DEG C/min's Heating rate is heated to 800 DEG C, is cooled to room temperature after keeping 90min.
The product obtained by the present embodiment is Fe-Fe3O4Biological carbon, Fe3+Fe is mainly reduced into.
Embodiment 5:
Cocoanut husk powder iron chloride viscous mixture is added to silica crucible to be put in tube furnace boiler tube, evacuation 10min, logical 200 DEG C are heated to the heating rate of 5 DEG C/min under conditions of nitrogen protection after nitrogen 10min, afterwards with 10 DEG C/min's Heating rate is heated to 800 DEG C, is cooled to room temperature after keeping 2h.
The product obtained by the present embodiment is Fe-Fe3O4Biological carbon, Fe3+Fe is mainly reduced into.
Embodiment 6:
Cocoanut husk powder iron chloride viscous mixture is added to silica crucible to be put in tube furnace boiler tube, evacuation 10min, logical 200 DEG C are heated to the heating rate of 5 DEG C/min under conditions of nitrogen protection after nitrogen 10min, afterwards with 10 DEG C/min's Heating rate is heated to 800 DEG C, is cooled to room temperature after keeping 3h.
The product obtained by the present embodiment is high-purity Fe biological carbon.
Embodiment 7:
Cocoanut husk is exposed to the sun, is dried, crush after cross 200 mesh sieve, take FeCl3·6H2O 30g are dissolved in dehydrated alcohol, 200 mesh cocoanut husk powder 12g are added, after stirring 24h, 30 days is stood.By cocoanut husk powder iron chloride alcohol mixed solution upper liquid Body is poured out, and after revolving reclaims big portion's ethanol, solution refunds stirring 5h, dries complete to moisture after standing 2 days under conditions of 100 DEG C Full volatilization.Cocoanut husk powder iron chloride mixture is added to silica crucible to be put in tube furnace boiler tube, evacuation 10min, logical 200 DEG C are heated to the heating rate of 5 DEG C/min under conditions of nitrogen protection after nitrogen 10min, afterwards with 10 DEG C/min's Heating rate is heated to 800 DEG C, is cooled to room temperature after keeping 3h.
The product obtained by the present embodiment is Fe3C biological carbons.
Embodiment 8:
Cocoanut husk powder iron chloride viscous mixture is added to silica crucible to be put in tube furnace boiler tube, evacuation 10min, logical 200 DEG C are heated to the heating rate of 5 DEG C/min under conditions of nitrogen protection after nitrogen 10min, afterwards with 15 DEG C/min's Heating rate is heated to 800 DEG C, is cooled to room temperature after keeping 4h.
The product obtained by the present embodiment is high-purity Fe biological carbon.
Embodiment 9:
Cocoanut husk powder iron chloride viscous mixture is added to silica crucible to be put in tube furnace boiler tube, evacuation 10min, logical 200 DEG C are heated to the heating rate of 3 DEG C/min under conditions of helium protection after helium 10min, afterwards with 10 DEG C/min's Heating rate is heated to 800 DEG C, is cooled to room temperature after keeping 4h.
The product obtained by the present embodiment is high-purity Fe biological carbon.
Embodiment 10:
100 mesh sieve are crossed after Cocos nucifera L. petiole is exposed to the sun, is dried, being crushed and makes powder, take Fe (NO3)3·9H2O 20g are dissolved in nothing In water-ethanol, cocoanut husk powder 8g is added, 20 days is stood after stirring 20h, by cocoanut husk powder ferric nitrate alcohol mixeding liquid upper strata Liquid is poured out, and after revolving reclaims most of ethanol, solution refunds stirring 3h, after standing 2 days, is dried to viscous under conditions of 100 DEG C Thick state, mixture of viscous form is added in tube furnace, after evacuation 5min, logical nitrogen 5min under conditions of nitrogen protection 200 DEG C are heated to the heating rate of 5 DEG C/min, 800 DEG C are heated to the heating rate of 10 DEG C/min afterwards, cold after holding 3h But room temperature is arrived.
The product obtained by the present embodiment is high-purity Fe biological carbon.
Embodiment 11:
150 mesh sieve are crossed after palm petiole is exposed to the sun, is dried, being crushed and makes powder, takeFe 2 (SO 4 ) 3 ·5H 2 O 40g are dissolved in In dehydrated alcohol, cocoanut husk powder 18g stands 40 days after stirring 30h, cocoanut husk powderFe 2 (SO 4 ) 3 ·5H 2 O alcohol mixeding liquids Supernatant liquid is poured out, and after revolving reclaims most of ethanol, solution refunds stirring 10h, after standing 3 days, dries under conditions of 100 DEG C Do to viscous pasty state, mixture of viscous form is added in tube furnace, protect in nitrogen after evacuation 15min, logical nitrogen 15min Under conditions of be heated to 200 DEG C with the heating rate of 5 DEG C/min, be heated to 800 DEG C with the heating rate of 10 DEG C/min afterwards, protect Room temperature is cooled to after holding 3h.
The product obtained by the present embodiment is high-purity Fe biological carbon.

Claims (3)

1. a kind of high-purity Zero-valent Iron biological carbon preparation method, it is characterised in that step is as follows:
(1) 100~200 mesh sieve are crossed after first cocoanut husk, Cocos nucifera L. petiole, palm petiole being exposed to the sun, dried, being crushed Make powder;
(2) iron chloride, ferric nitrate or 20~40g of iron sulfate are taken to be dissolved in dehydrated alcohol, is added ~18g, stands 20~40 days after 20~30h of stirring;
(3) step (2) mixed solution supernatant liquid is poured out, after revolving reclaims most of ethanol, solution refunds 3~10h of stirring, After standing 2~3 days, dry to viscous pasty state under conditions of 100 DEG C;
(4) mixture of viscous form in step (3) is added in tube furnace, 5~15min of evacuation, logical nitrogen or helium 5~ 200 DEG C are heated to the heating rate of 3~5 DEG C/min under conditions of nitrogen or helium protection after 15min, afterwards with 10~15 DEG C/heating rate of min is heated to 800 DEG C, room temperature is cooled to after keeping 3~4h, high-purity Zero-valent Iron biological carbon is obtained.
2. a kind of high-purity Zero-valent Iron biological carbon preparation method according to claim 1, it is characterised in that:
(1) cross 200 mesh sieve to make after first cocoanut husk, Cocos nucifera L. petiole, palm petiole being exposed to the sun, dried, being crushed Powder;
(2) iron chloride, ferric nitrate or iron sulfate 30g are taken to be dissolved in dehydrated alcohol, is added in step (1) and is obtained powder 12g, stir 30 days are stood after mixing 24h;
(3) step (2) mixed solution supernatant liquid is poured out, after revolving reclaims most of ethanol, solution refunds stirring 5h, stands After 2 days, dry to viscous pasty state under conditions of 100 DEG C;
(4) mixture of viscous form in step (3) is added in tube furnace, in nitrogen after evacuation 10min, logical nitrogen 10min 200 DEG C are heated to the heating rate of 5 DEG C/min under conditions of protection, 800 are heated to the heating rate of 10 DEG C/min afterwards DEG C, room temperature is cooled to after keeping 3h, high-purity Zero-valent Iron biological carbon is obtained.
3. a kind of high-purity Zero-valent Iron biological carbon preparation method according to claim 1 and 2, it is characterised in that:Preparing Sharp reduction with carbon ferric ion during biological carbon.
CN201610906553.2A 2016-10-17 2016-10-17 A kind of high-purity Zero-valent Iron biological carbon preparation method Pending CN106493384A (en)

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CN108326323A (en) * 2018-03-29 2018-07-27 洛阳理工学院 A kind of preparation method of rice husk carbon load nanometer nulvalent iron particle
CN108854951A (en) * 2018-06-05 2018-11-23 南昌大学 The method that one-step method prepares charcoal nano zero valence iron nickel composite
CN110217775A (en) * 2019-06-27 2019-09-10 中冶南方都市环保工程技术股份有限公司 A kind of preparation method and applications of pickling ZVI modification biological charcoal
CN114471466A (en) * 2022-03-09 2022-05-13 西南交通大学 Amino-modified corncob derived nitrogen-doped nano zero-valent iron/charcoal and preparation method and application thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108326323A (en) * 2018-03-29 2018-07-27 洛阳理工学院 A kind of preparation method of rice husk carbon load nanometer nulvalent iron particle
CN108854951A (en) * 2018-06-05 2018-11-23 南昌大学 The method that one-step method prepares charcoal nano zero valence iron nickel composite
CN108854951B (en) * 2018-06-05 2021-04-02 南昌大学 Method for preparing biochar nano zero-valent iron-nickel compound by one-step method
CN110217775A (en) * 2019-06-27 2019-09-10 中冶南方都市环保工程技术股份有限公司 A kind of preparation method and applications of pickling ZVI modification biological charcoal
CN114471466A (en) * 2022-03-09 2022-05-13 西南交通大学 Amino-modified corncob derived nitrogen-doped nano zero-valent iron/charcoal and preparation method and application thereof

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Application publication date: 20170315