CN105399872A - Method for using pennisetum hydridum lignin for preparation of active carbon and application of active carbon - Google Patents
Method for using pennisetum hydridum lignin for preparation of active carbon and application of active carbon Download PDFInfo
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- CN105399872A CN105399872A CN201510973677.8A CN201510973677A CN105399872A CN 105399872 A CN105399872 A CN 105399872A CN 201510973677 A CN201510973677 A CN 201510973677A CN 105399872 A CN105399872 A CN 105399872A
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- huge bacterium
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229920005610 lignin Polymers 0.000 title claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 title abstract description 13
- 241000209046 Pennisetum Species 0.000 title abstract 5
- 239000000571 coke Substances 0.000 claims abstract description 50
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000001784 detoxification Methods 0.000 claims abstract description 32
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 241000894006 Bacteria Species 0.000 claims description 81
- 239000000243 solution Substances 0.000 claims description 64
- 244000025254 Cannabis sativa Species 0.000 claims description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- 229920002488 Hemicellulose Polymers 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 238000007598 dipping method Methods 0.000 claims description 25
- 239000000706 filtrate Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 20
- 238000004061 bleaching Methods 0.000 claims description 19
- 239000001913 cellulose Substances 0.000 claims description 16
- 229920002678 cellulose Polymers 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 14
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 13
- 230000004913 activation Effects 0.000 claims description 13
- 238000001994 activation Methods 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- 235000012054 meals Nutrition 0.000 claims description 9
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 9
- 238000002203 pretreatment Methods 0.000 claims description 9
- 230000037452 priming Effects 0.000 claims description 9
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 7
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000000811 xylitol Substances 0.000 claims description 7
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 7
- 229960002675 xylitol Drugs 0.000 claims description 7
- 235000010447 xylitol Nutrition 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000003809 water extraction Methods 0.000 claims description 6
- SRBFZHDQGSBBOR-LECHCGJUSA-N alpha-D-xylose Chemical compound O[C@@H]1CO[C@H](O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-LECHCGJUSA-N 0.000 claims description 5
- 239000010902 straw Substances 0.000 claims description 5
- FRPJTGXMTIIFIT-UHFFFAOYSA-N tetraacetylethylenediamine Chemical compound CC(=O)C(N)(C(C)=O)C(N)(C(C)=O)C(C)=O FRPJTGXMTIIFIT-UHFFFAOYSA-N 0.000 claims description 5
- 229960003487 xylose Drugs 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 4
- 238000000855 fermentation Methods 0.000 claims description 4
- 230000004151 fermentation Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 abstract description 12
- 238000004042 decolorization Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 10
- 239000002699 waste material Substances 0.000 abstract description 6
- 230000007062 hydrolysis Effects 0.000 abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 5
- 238000003763 carbonization Methods 0.000 abstract 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 24
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 16
- 239000008367 deionised water Substances 0.000 description 15
- 229910021641 deionized water Inorganic materials 0.000 description 15
- 150000002989 phenols Chemical class 0.000 description 13
- 238000003756 stirring Methods 0.000 description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 238000005470 impregnation Methods 0.000 description 8
- 230000007935 neutral effect Effects 0.000 description 8
- 230000035484 reaction time Effects 0.000 description 8
- 229910019142 PO4 Inorganic materials 0.000 description 7
- 238000009835 boiling Methods 0.000 description 7
- 239000004570 mortar (masonry) Substances 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 7
- 239000010452 phosphate Substances 0.000 description 7
- 238000010792 warming Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000011010 flushing procedure Methods 0.000 description 5
- 239000000049 pigment Substances 0.000 description 5
- 239000000376 reactant Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- VEVZSMAEJFVWIL-UHFFFAOYSA-O cyanidin cation Chemical compound [O+]=1C2=CC(O)=CC(O)=C2C=C(O)C=1C1=CC=C(O)C(O)=C1 VEVZSMAEJFVWIL-UHFFFAOYSA-O 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000001814 pectin Substances 0.000 description 2
- 229920001277 pectin Polymers 0.000 description 2
- 235000010987 pectin Nutrition 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000010200 validation analysis Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- MIDXCONKKJTLDX-UHFFFAOYSA-N 3,5-dimethylcyclopentane-1,2-dione Chemical compound CC1CC(C)C(=O)C1=O MIDXCONKKJTLDX-UHFFFAOYSA-N 0.000 description 1
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- 241001672212 Cenchrus purpureus Species 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 235000019750 Crude protein Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000510612 Imperatoria Species 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 229920002522 Wood fibre Polymers 0.000 description 1
- 238000011481 absorbance measurement Methods 0.000 description 1
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- SRBFZHDQGSBBOR-QMKXCQHVSA-N alpha-L-arabinopyranose Chemical compound O[C@H]1CO[C@@H](O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-QMKXCQHVSA-N 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013736 caramel Nutrition 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000007336 cyanidin Nutrition 0.000 description 1
- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011094 fiberboard Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/14—Hemicellulose; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Health & Medical Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The present invention discloses a method for using pennisetum hydridum lignin for preparation of active carbon and application of the active carbon, the method comprises the following steps: hydrothermal coke can be prepared from the pennisetum hydridum lignin as a raw material by a hydrothermal method, the hydrothermal coke is impregnated with a solution of phosphoric acid, then the impregnated hydrothermal coke is put into a muffle furnace for carbonization, and finally the impregnated hydrothermal after the carbonization is activated by a hydrochloric acid solution, washed and dried to obtain the active carbon. The active carbon prepared from a pennisetum hydridum waste residue is just suitable for detoxification and decoloration of a hydrolyzate after pennisetum hydridum hydrolysis due to the pore size of the active carbon, and compared with the decolorization effect of purchased commodity active carbon, the decolorization effect of the active carbon is better.
Description
Technical field
The invention belongs to gac preparation field, be specifically related to a kind ofly utilize the huge bacterium grass method of Preparation of Activated Carbon with Lignin and gac thereof and application.
Background technology
Gac is because have more much higher permeability, and the features such as stronger adsorptive power and easy recycling are widely used in industrial circle.Huge bacterium grass has another name called imperatoria, hybrid giant napier, huge napier grass, is also referred to as generating grass, energy grass.This grass has fast growth, and plant is tall and big, and output is high, perennial etc., is the tropical pasture that China's output is the highest.After testing, vegetative period, the huge bacterium straw fiber cellulose content more than half a year can reach 25-43%, and hemicellulose level can reach 20-32%, content of lignin 10-13%, is therefore a kind of excellent fiber biomass.At present, huge bacterium is mainly used as culture medium of mushroom, cattle and sheep feed, biomass fuel generates electricity or for fiberboard manufacture etc., its abundant wood fibre does not obtain higher value application.
Summary of the invention
The invention provides a kind of method utilizing huge bacterium grass Preparation of Activated Carbon with Lignin, the aperture of gac prepared by this huge bacterium grass waste residue is just in time applicable to the detoxification decolouring of the hydrolyzed solution after the hydrolysis of huge bacterium grass, more excellent compared with the decolorizing effect of its merchandise active carbon bought.
The present invention is by the following technical solutions:
Huge bacterium vegetation quality is preparing an application for gac, and the preparation technology of described huge bacterium vegetation quality is that adopt benzene-ol, hot-water extraction pre-treatment, drying obtains huge bacterium grass meal with huge bacterium grass for raw material; And then adopt microwave-alkali-ol method to extract huge bacterium straw fiber element, hemicellulose and xylogen respectively, prepare hydrolyzed solution after wherein extracting hemicellulose, described hydrolyzed solution contains hemicellulose resolvent, and hydrolyzed solution prepares Xylitol through fermentation.
Wherein, described benzene-ol, the pretreated concrete steps of hot-water extraction are: in huge bacterium grass, add benzene-ol mixed solution extracting 5 ~ 7h dewax, be 1:(20-30 in mass ratio in the huge bacterium grass after dewaxing) add water, 80-90 DEG C is extracted 2-4h, filter, drying, obtains pretreated huge bacterium grass.
Preferably, the volume of described benzene-ol mixed solution and the quality of huge bacterium grass are (10 ~ 15) mL:10g.Described benzene-ol mixed solution is toluene and ethanol is (1.5-3) by volume: the solution of 1 mixing; Preferred further, described benzene-ol mixed solution is toluene and ethanol is the solution of 2:1 mixing by volume.
Huge bacterium grassland material is after pre-treatment, and most of wax, protein and pectin etc. are removed, and remaining material is mainly Mierocrystalline cellulose, hemicellulose and xylogen.
The leaching process of described xylogen is specific as follows: in pretreated huge bacterium grass, add NaOH-H successively
2o
2mixing solutions and tetraacetyl ethylene diamine, microwave heating: 55-95 DEG C of process 1-4h, filter, filter residue and drying, is Mierocrystalline cellulose; After adjustment extraction Mierocrystalline cellulose, the pH to 5.0-5.5 of filtrate, adds ethanol, is settled out hemicellulose, centrifugation, namely obtain hemicellulose; Reclaim centrifugal after supernatant liquor in ethanol, regulate the pH to 1.5-2.5 reclaiming raffinate after ethanol, centrifugation, namely obtains xylogen.
Preferably, described NaOH-H
2o
2in mixing solutions, the mass concentration of NaOH is 1-4%, H
2o
2mass concentration be 0.1-0.5%.NaOH-H
2o
2mixing solutions is (15-25) ml:1g with the ratio of pretreated huge bacterium grass add-on.The add-on of tetraacetyl ethylene diamine is the quality of huge bacterium grass meal (over dry) after 1-3% pre-treatment.Before ethanol adds, first filtrate is concentrated, be concentrated into the 1/2-1/3 of former filtrate volume; In the filtrate after concentrated, add ethanol again, the add-on of ethanol be concentrated after filtrate volume 3-4 doubly.
A kind of method utilizing huge bacterium grass Preparation of Activated Carbon with Lignin, comprise the following steps: huge bacterium vegetation quality is mixed with water, hydrothermal method is adopted to prepare hydro-thermal coke, phosphoric acid solution is adopted to flood hydro-thermal coke again, then the hydro-thermal coke after dipping is put into muffle furnace to carbonize, finally adopt hydrochloric acid soln to activate the hydro-thermal coke after charing, washing, drying, obtains gac.
Huge bacterium vegetation quality in the present invention can adopt ordinary method to prepare, and preferably, adopts scheme described above to prepare.
Specifically comprise the following steps:
(1) preparation of hydro-thermal coke:
Huge bacterium vegetation quality mixed in a kettle. according to liquid ratio 8 ~ 12:1 and water, the reactor of sealing is full of nitrogen, is heated to 240 ~ 260 DEG C of insulation 3.5 ~ 4.5h, after insulation terminates, and cooling, washing, the solid obtained carries out drying and obtains hydro-thermal coke;
(2) hydro-thermal coke is flooded: adopt the hydro-thermal coke in phosphoric acid solution impregnation steps (2), wherein phosphoric acid solution is 2 ~ 4:1 with water coke quality ratio, and dipping time is 1 ~ 2h, after dipping terminates, the hydro-thermal coke of dipping is dry;
(3) carbonize hydro-thermal coke: dried hydro-thermal coke is put into muffle furnace, rises to 350 ~ 500 DEG C, priming reaction 0.5 ~ 1.5h with 10 ~ 12 DEG C/min heat-up rate, activation terminates rear cooling, and activation and process of cooling are carried out in nitrogen atmosphere;
(4) by the solid abrasive in step (3), after adopting HCl solution to activate powdered active carbon and get final product.
In step (1), preferably, described liquid ratio is 10:1, and temperature of reaction is 250 DEG C, and soaking time is 4h.Drying temperature is 105 DEG C, and time of drying is 24h.Through lot of experiment validation and analysis, the gac yield adopting above-mentioned condition to prepare is high, good decoloring performance.
The concrete steps of described washing are: by reactant filter first with massfraction be 95% ethanolic soln rinse 2-3 time, afterwards use again water flushing colourless to filtrate.
In step (2), the massfraction of described phosphoric acid solution is 75 ~ 85%, and described drying temperature is 90 DEG C.
In step (3), preferably, described heat-up rate is 10 DEG C/min.Through lot of experiment validation and analysis, the gac yield adopting above-mentioned condition to prepare is high, good decoloring performance.
In step (4), seethe with excitement the gac in step (3) in the HCl solution of 0.8 ~ 1.1mol/L (preferred 1mol/L) 1 ~ 1.5h (preferred 1h), rinse filtrate in neutral with water afterwards, namely obtain activated carbon at 100 ~ 110 DEG C of drying 6 ~ 12h (preferably 105 DEG C and 8h).The aperture of the gac after overactivation is substantially constant, but specific surface area improves about 30%, strengthens the detoxification decolorizing effect of huge bacterium grass hydrolyzed solution.
The gac that the present invention also provides a kind of described method to prepare, specific surface area and the total pore volume of gained gac reach 1600-1980m respectively
2/ g and 1.0-1.23cm
3/ g, aperture is 5 ~ 30nm.Application in the detoxification decolorization of the hydrolyzed solution of described gac after the hydrolysis of huge bacterium grass, described gac carries out decolouring detoxification to the above-mentioned hydrolyzed solution containing hemicellulose resolvent.
Bleaching process is the master operation that Xylitol is produced, the pigment that pigment in hydrolyzed solution has the natural pigment in raw material and generates aborning, natural pigment such as cyanidin(e) exists with glycoside, a sugar and a non-saccharide body can be hydrolyzed in acidic medium, in green in alkalescence, also produce nitrogenous coloring matter when protein and acid hydrolysis, carbohydrate also decomposes generation pigment in alkalescence, also can produce caramel colour during sugar heating.These factors all can make the color and luster of hydrolyzed solution deepen, and affect the quality of xylitol products, must carry out desolventing technology.The activated carbon of the decoloring ability of gac normally unit volume can take off the blue solution of methyl of how many volumes routinely, and can not test by this traditional method for the gac of Xylitol hydrolyzate decolorizing, must compare by the ability of gac Direct Dehydration solution liquid aborning, measure the quality of activated carbon quality.
Hemicellulose can contain the hemicellulose hydrolysate of the monose such as wood sugar, pectinose through hydrolysis, can be used for fermentable and obtains Xylitol, ethanol and other useful products.But in hydrolytic process, also create the toxicant that a certain amount of furfural, acetic acid, phenols etc. suppress hydrolyzed solution fermentation.How before fermentation to hydrolyzed solution pre-treatment detoxification, to improving hydrolyzed solution leavening property, to carry high product yield extremely important.
The present invention also provides a kind of decolouring detoxification process, comprise the following steps: the gac described in employing carries out decolouring detoxification to the above-mentioned hydrolyzed solution containing hemicellulose resolvent, the addition of gac is 0.1% ~ 1% of hydrolyzed solution quality, bleaching temperature is 30 ~ 40 DEG C, and bleaching time is 1.5 ~ 3h.
The invention has the beneficial effects as follows:
(1) Mierocrystalline cellulose, hemicellulose and xylogen itself is all the macromolecular compounds with Complicated Spatial Structure; in natural cellulosic feedstocks; their polymerizations are as a whole; form complicated super molecular compound. wherein; xylogen major part is present in middle lamella; form mortise layer with hemicellulose, covering protection effect is formed to Mierocrystalline cellulose.Employing benzene-ol, hot-water extraction carry out pre-treatment to huge bacterium grass, then adopt microwave-alkali-ol method to extract huge bacterium straw fiber element, hemicellulose and xylogen respectively, and microwave refers to the hertzian wave of range of frequency at 300MHz ~ 300GHz.Microwave radiation exaraction is the impact utilizing microwave radiation to produce molecular motion, promote intermolecular friction and collision, when adopting microwave treatment, huge bacterium grassland can be made to expect lignin degrading and hemicellulose, the chemical reaction of the huge bacterium grass of effective raising, shortens the reaction times greatly, enhances productivity.Adopt the huge bacterium grass of alkaline purification, weak base destroys the chemical bonds between xylogen and polysaccharide, makes Mierocrystalline cellulose and lignin separation, insoluble xylogen is become more molten hydroxyl xylogen, crystalline cellulose becomes amorphous cellulose, causes cell expansion, makes huge bacterium grass structure become loose; Further, in alkaline purification process, in huge bacterium grass, the content of crude protein significantly improves, and can improve amido functional group quantity.Huge bacterium grass is carried out microwave-alkali-ol process, effectively can strengthen dipping effect, improve the specific surface area of gac, and form the gac with certain pore size size.To sum up, adopt benzene-ol, hot-water extraction carries out pre-treatment to huge bacterium grass, then adopt microwave-alkali-ol method to extract huge bacterium vegetation quality, and the gac having certain application performance for preparation provides a good basis.
(2) first the present invention adopts hydrothermal method to prepare coke, makes activated carbon surface have abundant functional group, and these surface groups make gac have good wetting ability, thus improves the adsorptive power of gac.
(3) the huge bacterium vegetation quality preparation after the present invention utilizes extraction hemicellulose, Mierocrystalline cellulose has the gac of certain performance, pore texture is flourishing, its pick-up rate is higher, reach 38 ~ 41%, specific surface area is carried out to gained gac and total pore volume measures, reach 1600-1980m respectively
2/ g and 1.0-1.23cm
3/ g, aperture is 5 ~ 30nm, and simultaneously the unexpected aperture finding that gac prepared by this huge bacterium vegetation quality waste residue is just in time applicable to the detoxification decolouring of the hydrolyzed solution after the hydrolysis of huge bacterium grass, and effect is very excellent, meets the application request of enterprises.
In addition, the shortcoming of gac adopting traditional material (coconut husk, nut-shell, bamboo etc.) to manufacture is that the consumption of the chemical reagent amount such as energy consumption, phosphoric acid of activator and water is large, and the rate of recovery is low, and the waste water and gas of generation causes certain harm to environment.The characteristic of hemicellulose, cellulosic huge bacterium grass waste residue is extracted according to the present invention; the phosphoric acid consumption that the present invention adopts is at 1.0-1.4% (preparing the acid consumption of every kg gac); phosphoric acid consumption is considerably less; the rate of recovery of residue phosphoric acid can reach more than 99%; and be comparatively low-temperature activation; do not need higher temperatures; the low consumption of phosphoric acid and comparatively low-temperature activation not only reduce production cost and energy consumption greatly; and protect environment; realize the cleaner production of enterprises, also achieve the high-qualityization complete utilization of huge bacterium grass.
(4) the present invention adopts a kind of distinctive waste material in enterprise; meet application request; realize internal enterprise resources circulationization; realize the comprehensive reutilization of refuse; improve enterprise's production level; save energy, clean resource, protect environment, meet the relevant policies regulation of country.
(5) invention adopts simple chemicals logos, huge bacterium grass waste residue after extracting hemicellulose is prepared into powdered active carbon, for extracting decolouring detoxification when hemicellulose prepares xylo-oligosaccharide from the material of huge bacterium grassland, so both achieved the high-valued complete utilization of huge bacterium grassland material, again reduce enterprise's production cost, realize energy-saving and emission-reduction.The present invention prepares in gac process, and the rate of recovery of phosphoric acid can reach more than 99%, thus no acidic waste water, exhaust gas emission, meet national energy-saving environmental protection policy.
Embodiment
Embodiment 1
The huge bacterium of 40-60 object carelessly powder is obtained through sub-sieve screening with benzene-ol, hot-water extraction pre-treatment.Huge bacterium straw fiber element, hemicellulose and xylogen is extracted respectively by microwave-alkali-ol method.
Concrete extraction step is as follows: (1) raw materials pretreatment: by broken for air-dry huge bacterium grass meal, 40-60 object grass meal is obtained through sub-sieve screening, 150mL benzene-ol mixed solution is added in Soxhlet extractor, dewax to carrying out extracting 5-7h in huge bacterium grass meal, be 1:(20-30 in mass ratio in the huge bacterium grass after dewaxing) add water, wherein the quality of huge bacterium grass is 10g, 80-90 DEG C is extracted 2-4h, the material such as protein and pectin in the huge bacterium grass of further removing, filter, dry, obtain pretreated huge bacterium grass, then cross 40 ~ 60 mesh sieve and obtain huge bacterium grass meal.
Wherein, described benzene-ol mixed solution is toluene and ethanol is the solution of 2:1 mixing by volume.
(2) extraction of Mierocrystalline cellulose, hemicellulose and xylogen: add NaOH-H successively in pretreated huge bacterium grass meal
2o
2mixing solutions and tetraacetyl ethylene diamine, use microwave chemical reaction producer, and be heated to 55-95 DEG C of process 1-4h, filter, filter residue and drying, is Mierocrystalline cellulose; After adjustment extraction Mierocrystalline cellulose, the pH to 5.0-5.5 of filtrate, adds ethanol, is settled out hemicellulose, centrifugation, namely obtain hemicellulose; Reclaim centrifugal after supernatant liquor in ethanol, regulate the pH to 1.5-2.5 reclaiming raffinate after ethanol, centrifugation, namely obtains xylogen.
Described NaOH-H
2o
2in mixing solutions, the mass concentration of NaOH is 1-4%, H
2o
2mass concentration be 0.1-0.5%.NaOH-H
2o
2mixing solutions is (15-25) ml:1g with the ratio of pretreated huge bacterium grass add-on.The add-on of tetraacetyl ethylene diamine is the quality of huge bacterium grass meal (over dry) after 1-3% pre-treatment.Before ethanol adds, first filtrate is concentrated, be concentrated into the 1/2-1/3 of former filtrate volume; In the filtrate after concentrated, add ethanol again, the add-on of ethanol be concentrated after filtrate volume 3-4 doubly.
The purity of xylogen is 86.4-93.3% after measured.
The huge bacterium vegetation quality taking 5g separating obtained fully mixes with deionized water according to liquid ratio 10:1 in 250mLParr reactor, passes into the air in nitrogen discharge reactor in the reactor of sealing.Reactor is heated to 250 DEG C, 150rpm stirs insulation 4 hours.After 4 hours, reactor cold water is cooled to room temperature rapidly.Reactant is filtered and first uses 95% alcohol flushing 2 times, more colourless to filtrate with deionized water rinsing, finally gained solid dry 24h at 105 DEG C is obtained hydro-thermal coke.
With 85% phosphate impregnation hydro-thermal coke obtained above, impregnating ratio is 3:1.Abundant stirring dipping, after 2 hours, is dried at 90 DEG C, the hydro-thermal coke of dipping.Drying object is transferred in tube type resistance furnace, is warming up to 400 DEG C with 10 DEG C/min heat-up rate, priming reaction 1 hour.Room temperature is naturally cooled to after reaching the reaction times.Whole activation and process of cooling are carried out in nitrogen atmosphere.After gained solid grinds in mortar, when boiling with the HCl solution of 1mol/L, activate 1h, filter, with deionized water, filtrate washing is extremely neutral, obtain gac at 105 DEG C of dry 12h.Its specific surface area and total pore volume reach maximum, are respectively 1980m
2/ g and 1.23cm
3/ g, aperture is 5 ~ 30nm, and the yield of activated carbon is 39.2%, and phosphoric acid consumption is 1%.
During by the decolouring detoxification of the huge bacterium grass hydrolyzed solution of this activated carbon application after extracting hemicellulose, the addition of gac is 0.5% of hydrolyzed solution quality, bleaching temperature is 35 DEG C, bleaching time is 1.5h, and decolouring detoxification efficiency is excellent, wherein, percent of decolourization is 95.8%, acetic acid clearance is 96.4%, and furfural clearance is 99%, phenolic compound removal efficiency R
280value 0.003, wood sugar rate of loss is less, is only 5.98%.
Embodiment 2
According to impregnating ratio 3:1, with 85% phosphate impregnation hydro-thermal coke (hydro-thermal coke preparation method is with example 1).Abundant stirring dipping, after 2 hours, is dried at 90 DEG C, the hydro-thermal coke of dipping.Drying object is transferred in tube type resistance furnace, is warming up to 450 DEG C with 10 DEG C/min heat-up rate, insulation priming reaction 1.5 hours.Room temperature is naturally cooled to after reaching the reaction times.Whole activation and process of cooling are carried out in nitrogen atmosphere.After gained solid grinds in mortar, when boiling with the HCl solution of 1mol/L, activate 1h, filter, with deionized water, filtrate washing is extremely neutral, obtain gac 105 DEG C of oven dry.Its specific surface area and total pore volume reach maximum, are respectively 1806m
2/ g and 1.12cm
3/ g, aperture is 5 ~ 30nm, and the yield of activated carbon is 40.5%, and phosphoric acid consumption is 1.2%.
During by the decolouring detoxification of the huge bacterium grass hydrolyzed solution of this activated carbon application after extracting hemicellulose, the addition of gac is 0.8% of hydrolyzed solution quality, bleaching temperature is 40 DEG C, bleaching time is 2h, and decolouring detoxification efficiency is excellent, wherein, percent of decolourization is 97.8%, acetic acid clearance is 97.4%, and furfural clearance is 99.5%, phenolic compound removal efficiency R
280value 0.004, wood sugar rate of loss is less, is only 5.88%.
Embodiment 3
According to impregnating ratio 2:1, with 75% phosphate impregnation hydro-thermal coke (hydro-thermal coke preparation method is with example 1).Abundant stirring dipping, after 1.5 hours, is dried at 90 DEG C, the hydro-thermal coke of dipping.Drying object is transferred in tube type resistance furnace, is warming up to 350 DEG C with 10 DEG C/min heat-up rate, insulation priming reaction 1.5 hours.Room temperature is naturally cooled to after reaching the reaction times.Whole activation and process of cooling are carried out in nitrogen atmosphere.After gained solid grinds in mortar, when boiling with the HCl solution of 1mol/L, activate 1h, filter, with deionized water, filtrate washing is extremely neutral, obtain gac 105 DEG C of oven dry.Its specific surface area and total pore volume reach maximum, are respectively 1756m
2/ g and 1.05cm
3/ g, aperture is 5 ~ 30nm, and the yield of activated carbon is 40.9%, and phosphoric acid consumption is 1.3%.
During by the decolouring detoxification of the huge bacterium grass hydrolyzed solution of this activated carbon application after extracting hemicellulose, the addition of gac is 1% of hydrolyzed solution quality, bleaching temperature is 37 DEG C, bleaching time is 1.5h, and decolouring detoxification efficiency is excellent, wherein, percent of decolourization is 98.9%, acetic acid clearance is 94.1%, and furfural clearance is 98.9%, phenolic compound removal efficiency R
280value 0.003, wood sugar rate of loss is less, is only 5.56%.
Comparative example 1
The huge bacterium vegetation quality taking 5g separating obtained fully mixes with deionized water according to liquid ratio 10:1 in 250mLParr reactor, passes into the air in nitrogen discharge reactor in the reactor of sealing.Reactor is heated to 200 DEG C, 150rpm stirs insulation 4 hours.After 4 hours, reactor cold water is cooled to room temperature rapidly.Reactant is filtered and first uses 95% alcohol flushing 2 times, more colourless to filtrate with deionized water rinsing, finally gained solid dry 24h at 105 DEG C is obtained hydro-thermal coke.
With 85% phosphate impregnation hydro-thermal coke obtained above, impregnating ratio is 3:1.Abundant stirring dipping, after 2 hours, is dried at 90 DEG C, the hydro-thermal coke of dipping.Drying object is transferred in tube type resistance furnace, is warming up to 400 DEG C with 10 DEG C/min heat-up rate, priming reaction 1 hour.Room temperature is naturally cooled to after reaching the reaction times.Whole activation and process of cooling are carried out in nitrogen atmosphere.After gained solid grinds in mortar, when boiling with the HCl solution of 1mol/L, activate 1h, filter, with deionized water, filtrate washing is extremely neutral, obtain gac at 105 DEG C of dry 12h.Its specific surface area and total pore volume reach 1480m
2/ g and 0.93cm
3/ g, aperture is 5 ~ 50nm, and the yield of activated carbon is 29.32%.
During by the decolouring detoxification of the huge bacterium grass hydrolyzed solution of this activated carbon application after extracting hemicellulose, the addition of gac is 0.5% of hydrolyzed solution quality, bleaching temperature is 35 DEG C, bleaching time is 1.5h, and decolouring detoxification efficiency is excellent, wherein, percent of decolourization is 63.25%, acetic acid clearance is 35.93%, and furfural clearance is 45.02%, phenolic compound removal efficiency R
280value 0.6.
The huge bacterium vegetation quality taking 5g separating obtained fully mixes with deionized water according to liquid ratio 10:1 in 250mLParr reactor, passes into the air in nitrogen discharge reactor in the reactor of sealing.Reactor is heated to 200 DEG C, 150rpm stirs insulation 4 hours.After 4 hours, reactor cold water is cooled to room temperature rapidly.Reactant is filtered and first uses 95% alcohol flushing 2 times, more colourless to filtrate with deionized water rinsing, finally gained solid dry 24h at 105 DEG C is obtained hydro-thermal coke.
Comparative example 2
The huge bacterium vegetation quality taking 5g separating obtained fully mixes with deionized water according to liquid ratio 10:1 in 250mLParr reactor, passes into the air in nitrogen discharge reactor in the reactor of sealing.Reactor is heated to 300 DEG C, 150rpm stirs insulation 4 hours.After 4 hours, reactor cold water is cooled to room temperature rapidly.Reactant is filtered and first uses 95% alcohol flushing 2 times, more colourless to filtrate with deionized water rinsing, finally gained solid dry 24h at 105 DEG C is obtained hydro-thermal coke.
With 85% phosphate impregnation hydro-thermal coke obtained above, impregnating ratio is 3:1.Abundant stirring dipping, after 2 hours, is dried at 90 DEG C, the hydro-thermal coke of dipping.Drying object is transferred in tube type resistance furnace, is warming up to 400 DEG C with 15 DEG C/min heat-up rate, priming reaction 1 hour.Room temperature is naturally cooled to after reaching the reaction times.Whole activation and process of cooling are carried out in nitrogen atmosphere.After gained solid grinds in mortar, when boiling with the HCl solution of 1mol/L, activate 1h, filter, with deionized water, filtrate washing is extremely neutral, obtain gac at 105 DEG C of dry 12h.Its specific surface area and total pore volume reach 1456m
2/ g and 0.91cm
3/ g, aperture is 5 ~ 150nm, and the yield of activated carbon is 26.37%.
During by the decolouring detoxification of the huge bacterium grass hydrolyzed solution of this activated carbon application after extracting hemicellulose, the addition of gac is 0.5% of hydrolyzed solution quality, bleaching temperature is 35 DEG C, bleaching time is 1.5h, and decolouring detoxification efficiency is excellent, wherein, percent of decolourization is 68.05%, acetic acid clearance is 34.23%, and furfural clearance is 44.09%, phenolic compound removal efficiency R
280value 0.5.
Comparative example 3
According to impregnating ratio 3:1, with 85% phosphate impregnation hydro-thermal coke (hydro-thermal coke preparation method is with example 1).Abundant stirring dipping, after 2 hours, is dried at 90 DEG C, the hydro-thermal coke of dipping.Drying object is transferred in tube type resistance furnace, is warming up to 550 DEG C with 10 DEG C/min heat-up rate, insulation priming reaction 1.5 hours.Room temperature is naturally cooled to after reaching the reaction times.Whole activation and process of cooling are carried out in nitrogen atmosphere.After gained solid grinds in mortar, when boiling with the HCl solution of 1mol/L, activate 1h, filter, with deionized water, filtrate washing is extremely neutral, obtain gac 105 DEG C of oven dry.Its specific surface area and total pore volume reach 1556m
2/ g and 0.98cm
3/ g, aperture is 5 ~ 150nm, and the yield of activated carbon is 25.39%.
During by the decolouring detoxification of the huge bacterium grass hydrolyzed solution of this activated carbon application after extracting hemicellulose, the addition of gac is 0.5% of hydrolyzed solution quality, bleaching temperature is 35 DEG C, bleaching time is 1.5h, and decolouring detoxification efficiency is excellent, wherein, percent of decolourization is 58.05%, acetic acid clearance is 25.23%, and furfural clearance is 44.06%, phenolic compound removal efficiency R
280value 0.6.
Comparative example 4
According to impregnating ratio 5:1, with 85% phosphate impregnation hydro-thermal coke (hydro-thermal coke preparation method is with example 1).Abundant stirring dipping, after 2 hours, is dried at 90 DEG C, the hydro-thermal coke of dipping.Drying object is transferred in tube type resistance furnace, is warming up to 550 DEG C with 10 DEG C/min heat-up rate, insulation priming reaction 1.5 hours.Room temperature is naturally cooled to after reaching the reaction times.Whole activation and process of cooling are carried out in nitrogen atmosphere.After gained solid grinds in mortar, when boiling with the HCl solution of 1mol/L, activate 1h, filter, with deionized water, filtrate washing is extremely neutral, obtain gac 105 DEG C of oven dry.Its specific surface area and total pore volume reach 1756m
2/ g and 1.0cm
3/ g, aperture is 5 ~ 300nm, and the yield of activated carbon is 20.45%.
During by the decolouring detoxification of the huge bacterium grass hydrolyzed solution of this activated carbon application after extracting hemicellulose, the addition of gac is 0.5% of hydrolyzed solution quality, bleaching temperature is 35 DEG C, bleaching time is 1.5h, and decolouring detoxification efficiency is excellent, wherein, percent of decolourization is 54.08%, acetic acid clearance is 24.29%, and furfural clearance is 45.03%, phenolic compound removal efficiency R
280value 0.8.
To sum up, can be drawn by above embodiment and comparative example, there is significant difference in the decolouring detoxification efficiency of different gacs, and through experimental verification and analysis, gac of the present invention is better compared with the decolorizing effect of the merchandise active carbon that it is bought.
Wherein, the mensuration of phenolic compound: carry out absorbance measurement at a wavelength of 280 nm to hydrolysising original liquid and detoxification liquid with UV-min1240 ultraviolet spectrophotometer, survey light absorption value after hydrolyzed solution and detoxification liquid distilled water diluting 100 times, distilled water is blank.According to following formula can be rough estimate the R of gac to phenolic compound
280value, this ratio represents the removal effect to phenolic compound, when ratio is 1, illustrates do not have removal effect to phenolic compound; Ratio is less, and the phenolic compound of removal is also more.R
280=detoxification liquid light absorption value/hydrolysising original liquid light absorption value.
Claims (10)
1. huge bacterium vegetation quality is preparing an application for gac, it is characterized in that: the preparation technology of described huge bacterium vegetation quality is that adopt benzene-ol, hot-water extraction pre-treatment, drying obtains huge bacterium grass meal with huge bacterium grass for raw material; And then adopt microwave-alkali-ol method to extract huge bacterium straw fiber element, hemicellulose and xylogen respectively, prepare hydrolyzed solution after wherein extracting hemicellulose, hydrolyzed solution prepares Xylitol through fermentation.
2. apply as claimed in claim 1, it is characterized in that: pretreated concrete steps are as follows: in huge bacterium grass, add benzene-ol mixed solution extracting 5 ~ 7h dewax, be 1:(20-30 in mass ratio in the huge bacterium grass after dewaxing) add water, 80-90 DEG C is extracted 2-4h, filter, drying, obtains pretreated huge bacterium grass.
3. apply as claimed in claim 3, it is characterized in that: the concrete steps extracting Mierocrystalline cellulose, hemicellulose and xylogen are: in pretreated huge bacterium grass, add NaOH-H successively
2o
2mixing solutions and tetraacetyl ethylene diamine, microwave heating, to 55-95 DEG C of process 1-4h, is filtered, is extracted Mierocrystalline cellulose; After adjustment extraction Mierocrystalline cellulose, the pH to 5.0-5.5 of filtrate, adds ethanol, is settled out hemicellulose, centrifugation; Reclaim centrifugal after supernatant liquor in ethanol, regulate the pH to 1.5-2.5 reclaiming raffinate after ethanol, centrifugation, namely obtains xylogen.
4. one kind utilizes the method for huge bacterium grass Preparation of Activated Carbon with Lignin, it is characterized in that, comprise the following steps: with huge bacterium vegetation quality for raw material, adopt hydrothermal method to prepare hydro-thermal coke, then adopt phosphoric acid solution to flood hydro-thermal coke, then the hydro-thermal coke after dipping is put into muffle furnace and carbonize, hydrochloric acid soln is finally adopted to activate the hydro-thermal coke after charing, washing, dry, obtain gac.
5. method as claimed in claim 4, it is characterized in that: the concrete steps that described hydrothermal method prepares hydro-thermal coke are as follows: huge bacterium vegetation quality is mixed in a kettle. according to liquid ratio 8 ~ 12:1 and water, the reactor of sealing is full of nitrogen, be heated to 240 ~ 260 DEG C of insulation 3.5 ~ 4.5h, after insulation terminates, cooling, washing, the solid obtained carries out drying and obtains hydro-thermal coke.
6. method as claimed in claim 4, it is characterized in that, the concrete steps of dipping hydro-thermal coke are as follows: adopt phosphoric acid solution dipping hydro-thermal coke, wherein phosphoric acid solution is 2 ~ 4:1 with water coke quality ratio, dipping time is 1 ~ 2h, after dipping terminates, the hydro-thermal coke of dipping is dry.
7. method as claimed in claim 4, it is characterized in that, the concrete steps of charing hydro-thermal coke are: dried hydro-thermal coke is put into muffle furnace, 350 ~ 500 DEG C are risen to 10 ~ 12 DEG C/min heat-up rate, priming reaction 0.5 ~ 1.5h, activation terminates rear cooling, and activation and process of cooling are carried out in nitrogen atmosphere.
8. the gac adopting the method according to any one of claim 4 ~ 7 to prepare.
9. gac according to claim 8 prepares the application in the decolouring During Detoxification of wood sugar and/or Xylitol technique at huge bacterium culm, it is characterized in that: described gac carries out decolouring detoxification to the hydrolyzed solution containing hemicellulose resolvent described in claim 1.
10. a decolouring detoxification process, it is characterized in that, comprise the following steps: adopt gac according to claim 8 to carry out decolouring detoxification to the hydrolyzed solution containing hemicellulose resolvent in claim 1, the addition of gac is 0.1% ~ 1% of hydrolyzed solution quality, bleaching temperature is 30 ~ 40 DEG C, and bleaching time is 1.5 ~ 3h.
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| CN105692611A (en) * | 2016-03-21 | 2016-06-22 | 中国科学院理化技术研究所 | Preparation method of biomass activated carbon rich in nitrogen and oxygen |
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| CN105923633A (en) * | 2016-04-22 | 2016-09-07 | 东北电力大学 | Method for reducing ash content in process of preparing activated carbon by using straws |
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