CN110237818A - A kind of preparation method and application of nitrogen sulphur codope charcoal - Google Patents
A kind of preparation method and application of nitrogen sulphur codope charcoal Download PDFInfo
- Publication number
- CN110237818A CN110237818A CN201910516949.XA CN201910516949A CN110237818A CN 110237818 A CN110237818 A CN 110237818A CN 201910516949 A CN201910516949 A CN 201910516949A CN 110237818 A CN110237818 A CN 110237818A
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- China
- Prior art keywords
- charcoal
- nitrogen sulphur
- nitrogen
- preparation
- sulphur codope
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- 239000003610 charcoal Substances 0.000 title claims abstract description 92
- PFRUBEOIWWEFOL-UHFFFAOYSA-N [N].[S] Chemical compound [N].[S] PFRUBEOIWWEFOL-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 27
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- -1 phthalic acid ester Chemical class 0.000 claims abstract description 12
- 238000000197 pyrolysis Methods 0.000 claims abstract description 12
- 239000005864 Sulphur Substances 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract 3
- 238000001816 cooling Methods 0.000 claims abstract 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 12
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 7
- 235000019394 potassium persulphate Nutrition 0.000 claims description 7
- 241001465754 Metazoa Species 0.000 claims description 6
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 5
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 4
- 244000105624 Arachis hypogaea Species 0.000 claims description 4
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 4
- 235000018262 Arachis monticola Nutrition 0.000 claims description 4
- 244000060011 Cocos nucifera Species 0.000 claims description 4
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 4
- 241000196324 Embryophyta Species 0.000 claims description 4
- 240000007594 Oryza sativa Species 0.000 claims description 4
- 235000007164 Oryza sativa Nutrition 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 4
- 235000018417 cysteine Nutrition 0.000 claims description 4
- 239000010903 husk Substances 0.000 claims description 4
- 235000020232 peanut Nutrition 0.000 claims description 4
- 235000009566 rice Nutrition 0.000 claims description 4
- 229940124530 sulfonamide Drugs 0.000 claims description 4
- 150000003456 sulfonamides Chemical class 0.000 claims description 4
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 3
- 240000008042 Zea mays Species 0.000 claims description 3
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 3
- 235000005822 corn Nutrition 0.000 claims description 3
- 239000010907 stover Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000002699 waste material Substances 0.000 claims description 2
- 230000009514 concussion Effects 0.000 claims 1
- 239000005416 organic matter Substances 0.000 claims 1
- 230000004048 modification Effects 0.000 abstract description 8
- 238000012986 modification Methods 0.000 abstract description 8
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 230000004913 activation Effects 0.000 abstract description 3
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 abstract 1
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 description 20
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 10
- 229910052717 sulfur Inorganic materials 0.000 description 9
- 239000011593 sulfur Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 230000008859 change Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 150000002148 esters Chemical class 0.000 description 5
- 235000019253 formic acid Nutrition 0.000 description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000004677 Nylon Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- DLGYNVMUCSTYDQ-UHFFFAOYSA-N azane;pyridine Chemical compound N.C1=CC=NC=C1 DLGYNVMUCSTYDQ-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 229920001778 nylon Polymers 0.000 description 4
- 230000010355 oscillation Effects 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 239000002689 soil Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 239000000499 gel Substances 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 150000003233 pyrroles Chemical class 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 230000008635 plant growth Effects 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 2
- DWNBOPVKNPVNQG-LURJTMIESA-N (2s)-4-hydroxy-2-(propylamino)butanoic acid Chemical compound CCCN[C@H](C(O)=O)CCO DWNBOPVKNPVNQG-LURJTMIESA-N 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000010828 animal waste Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- RXAVKZHNTOUUSP-UHFFFAOYSA-N dibutyl benzene-1,2-dicarboxylate;diethyl benzene-1,2-dicarboxylate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC.CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC RXAVKZHNTOUUSP-UHFFFAOYSA-N 0.000 description 1
- 229960002380 dibutyl phthalate Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000009656 pre-carbonization Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0271—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds also containing elements or functional groups covered by B01J31/0201 - B01J31/0231
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Hydrology & Water Resources (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to a kind of preparation method and application of nitrogen sulphur codope charcoal, carry out pyrolysis processing after biological carbon feedstock is crushed, and mesh screen is crossed after cooling；Nitrogen sulphur source is mixed, then nitrogen atmosphere calcination processing with charcoal, nitrogen sulphur codope charcoal is prepared.Compared with prior art, modification biological charcoal prepared by the present invention not only has good absorption property, moreover it is possible to pass through phthalic acid ester in activation persulfate efficient degradation water.The features such as modification biological charcoal of invention has raw material cheap and easy to get, and preparation process is simple, environmentally protective, the removal of organic pollutant suitable for water process.
Description
Technical field
The present invention relates to field of environment protection, a kind of preparation method more particularly, to nitrogen sulphur codope charcoal and answer
With.
Background technique
Charcoal be by high temperature pyrolysis organic substance, such as agricultural residue, animal waste or xylophyta, generation
Granular charcoal, and improvement environment aspect is produced and is applied to, soil is usually applied to improve soil property or storage
Carbon.Charcoal has large surface area, complicated pore structure and changeable surface composition, therefore is considered a kind of efficient
Adsorbent.Charcoal is nontoxic, harmless, and raw material is extensive, cheap, can largely prepare, and surface oxygen functional group is more, and easy surface changes
Property.It is modified to its surface with the method for nonmetal doping, the absorption property of Carbon Materials can not only be improved, can also be increased certainly
By the generation of base, there are catalysis potentiality, and preparation method is simple, operation is easy, and success rate is high, less energy consumption, for going to remove water
Organic pollutant phthalic acid ester effect in body is fine.
Sulphur plays the role of plant growth very important as the nutrient for being only second to nitrogen, phosphorus and potassium.Meanwhile sulphur
Plant growth regulating, removing toxic substances and it is degeneration-resistant etc. during also function to certain effect, be an important factor for influencing plant quality,
The importance of growth and metabolic process to plant is self-evident.Currently, the whole world about more than 70 the soil of a countries and regions deposit
The a lack of sulfur or potential a lack of sulfur the phenomenon that, a lack of sulfur can bring about great losses to agricultural production, to influence quality of agricultural product, and right
Ecological environment causes potential threat.The charcoal for the nitrogen sulfur doping being related in the present invention phthalic acid in effectively removing water
While this environmental contaminants of ester, unlimited potential also is provided for application in the soil.
Currently, the preparation and its application in organic pollutant removal that have not been reported nitrogen sulphur codope charcoal.For example,
Chinese patent CN109052364A discloses a kind of preparation method and application of porous nitrogen sulphur codope carbon nanosheet material of two dimension,
Preparation method includes the following steps: that (1) stirs gelatin with chitosan and foaming agent with certain proportion in 50~80 DEG C of water
The gel of formation is precipitated in excessive solidification liquid at gel and forms cavernous body by 0.1~2h；The foaming agent potassium carbonate, alkali
Formula magnesium carbonate or melamine；(2) gel that step (1) is formed is precipitated in excessive solidification liquid and forms cavernous body；Then
Cavernous body is placed in 330 DEG C~400 DEG C Muffle furnaces, heat preservation 0.5~4h of calcination processing carries out foaming and pre- carbonization, obtains pre- carbon
Change material；(3) the resulting pre- char-forming material of step (2) is ground uniformly with certain proportion and thiocarbamide, obtained mixture is existed
Calcination processing obtains the porous nitrogen sulphur codope carbon nanosheet material of two dimension under protective atmosphere.But the two dimension that the patent is prepared
Porous nitrogen sulphur codope carbon nanosheet is used primarily as lithium ion battery lithium anode protection materials.
Summary of the invention
It is raw that it is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of nitrogen sulphur codopes
The preparation method of object charcoal.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of nitrogen sulphur codope charcoal, comprising:
Pyrolysis processing is carried out after biological carbon feedstock is crushed, is then cooled down, obtained charcoal crosses mesh screen；
Nitrogen sulphur source is mixed, then calcination processing with charcoal, nitrogen sulphur codope charcoal is prepared.
Preferably, biological carbon feedstock is animals and plants waste.
It is further preferred that biological carbon feedstock includes peanut shell, rice husk, corn stover, cocoanut shell or animal excrements.
Preferably, the temperature control of pyrolysis is 200-700 DEG C, and the processing time is 1-3h, heating rate is 3-5 DEG C/min,
The above processing occurs under conditions of nitrogen protection, and stringent limitation cannot have oxygen.The charcoal handled through the above scheme
Surface can generate the new functional groups such as a large amount of sulfur oxide, thiophenic sulfur, pyrroles's nitrogen, pyridine nitrogen and graphene nitrogen, to the charcoal
Absorption and catalytic performance have very big facilitation.
Preferably, it is 100-300 mesh that charcoal, which crosses grit number,.
Preferably, nitrogen sulphur source includes thiocarbamide, cysteine ??acid, sulfonamide or thioacetamide.
Preferably, nitrogen sulphur source and charcoal mass ratio are 0.1-0.9.
Preferably, the temperature control of calcining is, not less than 350 DEG C or more, preferably 350 DEG C, is 1-3h, rises the processing time
Warm rate is 1-3 DEG C/min, and the above processing occurs to carry out under conditions of nitrogen protection.When temperature is controlled in the temperature range
It is interior, temperature is especially controlled to the substance decomposition that can make at 350 DEG C nitrogenous sulphur source, be supported on charcoal surface and hole it is interior
Portion.
Nitrogen sulphur codope charcoal, which is prepared, can be used for removing organic pollutant in water body, can be changed using this kind
Property charcoal remove plasticizer phthalic acid ester.
Preferably, phthalic acid ester removal experiment is carried out under conditions of 25 DEG C of isothermal vibrations.
Preferably, phthalic acid ester pH value of solution is 5-7.
Preferably, the removal effect of phthalic acid ester can reach 90% or more.
Compared with prior art, the invention has the following advantages that
1. the present invention is using agricultural wastes as raw material, preparation method is simple, low in cost；
2. charcoal is doped with nitrogen and element sulphur by the present invention, the existing forms of nitrogen have 3 kinds, are pyridine nitrogen, pyrroles respectively
Nitrogen and graphene nitrogen；The existing forms of sulphur have 2 kinds, are thiophenic sulfur respectively and the sulphur that is oxidized；The wherein sulphur of pyridine nitrogen and oxidation
Presence enhance the absorption property of modification biological charcoal, graphene nitrogen and thiophenic sulfur provide activation persulfuric acid for modification biological charcoal
The potentiality of salt.
3. the modification biological charcoal specific surface area that the present invention obtains is 1.46-28.28m2g-1, surface sulfur content is 0.5-
6.59%, nitrogen content 16.42-21.8%, by activating potassium peroxydisulfate, the removal rate of phthalic acid ester is reached as high as
96.75%；
4. the present invention realizes the substance by pyrolytic as nitrogen source sulphur source, by nitrogen and sulfur doping in charcoal,
Modified charcoal adsorption capacity also has phthalic acid ester in the water that can degrade by activation persulfate while enhancing
New capability.The present invention provides not only a kind of preparation method of charcoal nonmetal doping, is also useless containing phthalic acid ester
The improvement of water provides a kind of efficient material.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
A kind of preparation method of nitrogen sulphur codope charcoal, comprising:
(1) biological carbon feedstock, such as peanut shell, rice husk, corn stover, cocoanut shell or animal excrements etc. are crushed laggard
Row pyrolysis processing, control control heating rate is 3-5 DEG C/min in treatment process, and temperature is risen to 200-700 DEG C, handles 1-
Then 3h cools down, whole process, which strictly limits, cannot oxygen, carries out under conditions of nitrogen protection, so that being prepared
Biological carbon surface can generate the new functional groups such as a large amount of sulfur oxide, thiophenic sulfur, pyrroles's nitrogen, pyridine nitrogen and graphene nitrogen, it is right
The charcoal that the absorption of the charcoal and catalytic performance have very big facilitation to obtain crosses the mesh screen of 100-300 mesh；
(2) nitrogen sulphur source, such as thiocarbamide, cysteine ??acid, sulfonamide or thioacetamide are mixed with charcoal, nitrogen sulphur source with
Charcoal mass ratio is 0.1-0.9, then calcination processing, should control heating rate be in the process 1-3 DEG C/min, and be warming up to not low
In 350 DEG C of isothermal holding 1-3h, equally stringent limitation cannot there should be oxygen in the process, be carried out under conditions of nitrogen protection,
The substance decomposition for making nitrogenous sulphur source is supported on the surface of charcoal and the inside in hole, and nitrogen sulphur codope charcoal is prepared.
Nitrogen sulphur codope charcoal, which is prepared, can be used for removing organic pollutant in aqueous solution, can use this kind
Charcoal removes plasticizer phthalic acid ester.Removal experiment is carried out under conditions of 25 DEG C of isothermal vibrations, O-phthalic
Acid esters pH value of solution is 5-7, and removal effect can reach 90% or more.
More detailed case study on implementation below, by following case study on implementation further illustrate technical solution of the present invention with
And the technical effect that can be obtained.
Embodiment 1
A kind of preparation method of nitrogen sulphur codope charcoal, comprising:
(1) preparation of charcoal:
Peanut shell is cleaned up, with being placed in Muffle furnace for pulverizer coarse crushing, control heating rate be 4 DEG C/
Temperature is risen to 375 DEG C of pyrolysis 1h, Temperature fall by min, and the entire treatment process in Muffle furnace needs to control in nitrogen protection
Under atmosphere, burned charcoal is crossed to the mesh screen of 300 mesh.
(2) preparation of nitrogen sulphur codope charcoal:
Thiocarbamide and the charcoal for crossing mesh screen are uniformly mixed with the mass ratio of 0.1:1, heating rate is controlled in Muffle furnace
Temperature is risen into 350 DEG C of calcining 1h, Temperature fall for 2 DEG C/min, the entire treatment process in Muffle furnace needs to control in nitrogen
Under gas shielded atmosphere, deionized water clean the surface is then used, 60 DEG C are dried for standby.
(3) removal of diethyl phthalate
It is 20mg L that modified charcoal 100mg, which is added to the 20mL concentration containing 10mg potassium peroxydisulfate,-1Adjacent benzene two
In the brown conical flask of formic acid diethylester, ultrasonic 3min, 25 DEG C of constant temperature oscillations in constant temperature oscillator, reaction 2h sampling.By sample
Product measure phthalic acid diethyl in sample supernatant with high performance liquid chromatography after 0.22 μm of nylon filter filtering
The content of ester, calculating removal rate is 97.3%.
Embodiment 2
Embodiment 2 is the change case of embodiment 1, and variation place is that the cracking temperature of charcoal in step (1) is 200,
450,700 DEG C, removal rate is shown in Table 1.
Table 1
| Pyrolysis temperature (DEG C) | 200 | 450 | 700 |
| Diethyl phthalate removal rate (%) | 80.2 | 83.7 | 30.2 |
Embodiment 3
Embodiment 3 is the change case of embodiment 1, and variation place is that the mass ratio of step (2) thiocarbamide and charcoal is
0.3,0.5,0.7,0.9, removal rate is shown in Table 2.
Table 2
| The mass ratio of thiocarbamide and charcoal | 0.3 | 0.5 | 0.7 | 0.9 |
| Diethyl phthalate removal rate (%) | 83.7 | 45.8 | 30.6 | 20.3 |
Embodiment 4
Embodiment 4 is the change case of embodiment 1, and variation place is that the grit number of crossing of charcoal in step (1) is 100 Hes
200 mesh, removal rate are shown in Table 3.
Table 3
| Charcoal mesh number | 100 | 200 |
| Diethyl phthalate removal rate (%) | 83.7 | 92.8 |
Embodiment 5
Embodiment 5 is the change case of embodiment 1, and variation place is that step (1) charcoal was pyrolyzed the mesh screen of 300 mesh,
The removal of repefral and dibutyl phthalate is respectively used in step (3), removal rate is shown in Table 4.
Table 4
| Pollutant kind | Repefral | Diethyl phthalate | Dibutyl phthalate |
| Removal rate (%) | 93.3 | 96.7 | 85.6 |
Embodiment 6
Embodiment 6 is the change case of embodiment 1, and variation place is that step (2) changes half Guang into as the thiocarbamide of nitrogen sulphur source
One of propylhomoserin, sulfonamide or thioacetamide.
Table 5
Embodiment 7
A kind of preparation method of nitrogen sulphur codope charcoal, comprising:
(1) preparation of charcoal:
Rice husk is cleaned up, with being placed in Muffle furnace for pulverizer coarse crushing, control heating rate is 3 DEG C/min
Temperature is risen into 200 DEG C of pyrolysis 3h, Temperature fall, the entire treatment process in Muffle furnace needs to control in nitrogen protection atmosphere
Under, burned charcoal is crossed to the mesh screen of 100 mesh.
(2) preparation of nitrogen sulphur codope charcoal:
Cysteine ??acid and the charcoal for crossing mesh screen are uniformly mixed with the mass ratio of 0.5:1, heating is controlled in Muffle furnace
Temperature is risen to 400 DEG C of calcining 1h, Temperature fall for 1 DEG C/min by rate, and the entire treatment process in Muffle furnace needs to control
Under nitrogen protection atmosphere, deionized water clean the surface is then used, 60 DEG C are dried for standby.
(3) removal of diethyl phthalate
It is 20mg L that modified charcoal 100mg, which is added to the 20mL concentration containing 10mg potassium peroxydisulfate,-1Adjacent benzene two
In the brown conical flask of formic acid diethylester, ultrasonic 3min, 25 DEG C of constant temperature oscillations in constant temperature oscillator, reaction 2h sampling.By sample
Product measure phthalic acid diethyl in sample supernatant with high performance liquid chromatography after 0.22 μm of nylon filter filtering
The content of ester, calculating removal rate is 93.5%.
Embodiment 8
A kind of preparation method of nitrogen sulphur codope charcoal, comprising:
(1) preparation of charcoal:
Cocoanut shell is cleaned up, with being placed in Muffle furnace for pulverizer coarse crushing, control heating rate be 5 DEG C/
Temperature is risen to 600 DEG C of pyrolysis 2h, Temperature fall by min, and the entire treatment process in Muffle furnace needs to control in nitrogen protection
Under atmosphere, burned charcoal is crossed to the mesh screen of 200 mesh.
(2) preparation of nitrogen sulphur codope charcoal:
Thiocarbamide and the charcoal for crossing mesh screen are uniformly mixed with the mass ratio of 0.7:1, heating rate is controlled in Muffle furnace
Temperature is risen into 450 DEG C of calcining 2h, Temperature fall for 3 DEG C/min, the entire treatment process in Muffle furnace needs to control in nitrogen
Under gas shielded atmosphere, deionized water clean the surface is then used, 60 DEG C are dried for standby.
(3) removal of diethyl phthalate
It is 20mg L that modified charcoal 100mg, which is added to the 20mL concentration containing 10mg potassium peroxydisulfate,-1Adjacent benzene two
In the brown conical flask of formic acid diethylester, ultrasonic 3min, 25 DEG C of constant temperature oscillations in constant temperature oscillator, reaction 2h sampling.By sample
Product measure phthalic acid diethyl in sample supernatant with high performance liquid chromatography after 0.22 μm of nylon filter filtering
The content of ester, calculating removal rate is 92.5%.
Embodiment 9
A kind of preparation method of nitrogen sulphur codope charcoal, comprising:
(1) preparation of charcoal:
Animal excrements are cleaned up, with being placed in Muffle furnace for pulverizer coarse crushing, controlling heating rate is 5
DEG C/temperature rises to 700 DEG C of pyrolysis 1h by min, Temperature fall, the entire treatment process in Muffle furnace needs to control protects in nitrogen
It protects under atmosphere, burned charcoal is crossed to the mesh screen of 300 mesh.
(2) preparation of nitrogen sulphur codope charcoal:
Thioacetamide and the charcoal for crossing mesh screen are uniformly mixed with the mass ratio of 0.9:1, controls and rises in Muffle furnace
Temperature is risen to 350 DEG C of calcining 3h, Temperature fall for 3 DEG C/min by warm rate, and the entire treatment process in Muffle furnace needs to control
Then system uses deionized water clean the surface, 60 DEG C are dried for standby under nitrogen protection atmosphere.
(3) removal of diethyl phthalate
It is 20mg L that modified charcoal 100mg, which is added to the 20mL concentration containing 10mg potassium peroxydisulfate,-1Adjacent benzene two
In the brown conical flask of formic acid diethylester, ultrasonic 3min, 25 DEG C of constant temperature oscillations in constant temperature oscillator, reaction 2h sampling.By sample
Product measure phthalic acid diethyl in sample supernatant with high performance liquid chromatography after 0.22 μm of nylon filter filtering
The content of ester, calculating removal rate is 95.6%.
Comparative example 1
Comparative example 1 is the comparative example of embodiment 1, and comparison place is, does not carry out carrying out nitrogen sulphur to charcoal in step (2)
Codoping modified, diethyl phthalate removal rate is 20.3%, and the removal capacity of unmodified charcoal is co-doped with lower than nitrogen sulphur
The removal capacity of miscellaneous charcoal.
Comparative example 2
Comparative example 1 is the comparative example of embodiment 1, and comparison place is, potassium peroxydisulfate, adjacent benzene two are not added in step (3)
The removal rate of formic acid diethylester is 56.8%, and nitrogen sulphur codope charcoal has the function of activating persulfate.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (10)
1. a kind of preparation method of nitrogen sulphur codope charcoal, which is characterized in that this method comprises:
Pyrolysis processing is carried out after biological carbon feedstock is crushed, mesh screen is crossed after cooling；Nitrogen sulphur source is mixed with charcoal, then calcines place
Reason, is prepared nitrogen sulphur codope charcoal.
2. a kind of preparation method of nitrogen sulphur codope charcoal according to claim 1, which is characterized in that the charcoal
Raw material is animals and plants waste.
3. a kind of preparation method of nitrogen sulphur codope charcoal according to claim 1 or 2, which is characterized in that the life
Object carbon feedstock includes peanut shell, rice husk, corn stover, cocoanut shell or animal excrements.
4. a kind of preparation method of nitrogen sulphur codope charcoal according to claim 1, which is characterized in that the pyrolysis
Temperature control is 200-700 DEG C, and the processing time is 1-3h, heating rate is 3-5 DEG C/min, is carried out in a nitrogen atmosphere.
5. a kind of preparation method of nitrogen sulphur codope charcoal according to claim 1, which is characterized in that the charcoal
Crossing grit number is 100-300 mesh.
6. a kind of preparation method of nitrogen sulphur codope charcoal according to claim 1, which is characterized in that the nitrogen sulphur source
Including thiocarbamide, cysteine ??acid, sulfonamide or thioacetamide.
7. a kind of preparation method of nitrogen sulphur codope charcoal according to claim 1, which is characterized in that the nitrogen sulphur source
It is 0.1-0.9 with charcoal mass ratio.
8. a kind of preparation method of nitrogen sulphur codope charcoal according to claim 1, which is characterized in that the calcining
Temperature control is, not less than 350 DEG C, preferably 350 DEG C, the processing time is 1-3h, heating rate is 1-2 DEG C/min, the above processing
Process carries out under the conditions of nitrogen atmosphere.
9. nitrogen sulphur codope charcoal answering in Organic Pollutants In Water removal is prepared in method as described in claim 1
With.
10. a kind of application of nitrogen sulphur codope charcoal according to claim 9, which is characterized in that the nitrogen sulphur is co-doped with
Miscellaneous charcoal is added in the aqueous solution containing phthalic acid ester and a small amount of potassium peroxydisulfate, is placed in constant temperature oscillator, 25 DEG C of perseverances
Temperature concussion, adsorb and degrade organic matter therein.
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