CN117298670B - Sugar solution and lignin separation equipment and method in lignin preparation process by organic solvent method - Google Patents
Sugar solution and lignin separation equipment and method in lignin preparation process by organic solvent method Download PDFInfo
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- CN117298670B CN117298670B CN202311247094.8A CN202311247094A CN117298670B CN 117298670 B CN117298670 B CN 117298670B CN 202311247094 A CN202311247094 A CN 202311247094A CN 117298670 B CN117298670 B CN 117298670B
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- lignin
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- 229920005610 lignin Polymers 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 235000000346 sugar Nutrition 0.000 title claims abstract description 28
- 239000003960 organic solvent Substances 0.000 title claims abstract description 17
- 238000000926 separation method Methods 0.000 title claims abstract description 15
- 238000003825 pressing Methods 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 238000005406 washing Methods 0.000 claims abstract description 14
- 230000005540 biological transmission Effects 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 31
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000007787 solid Substances 0.000 claims description 25
- 239000003054 catalyst Substances 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000002131 composite material Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 239000001509 sodium citrate Substances 0.000 claims description 15
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- 238000011010 flushing procedure Methods 0.000 claims description 14
- 239000004408 titanium dioxide Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 239000004246 zinc acetate Substances 0.000 claims description 11
- 108010059892 Cellulase Proteins 0.000 claims description 10
- 229940106157 cellulase Drugs 0.000 claims description 10
- 239000012279 sodium borohydride Substances 0.000 claims description 10
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 10
- 239000004744 fabric Substances 0.000 claims description 7
- 240000008042 Zea mays Species 0.000 claims description 6
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 6
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 6
- 235000005822 corn Nutrition 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 3
- 230000000712 assembly Effects 0.000 claims 3
- 238000000429 assembly Methods 0.000 claims 3
- 230000006835 compression Effects 0.000 claims 1
- 238000007906 compression Methods 0.000 claims 1
- 230000006978 adaptation Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 14
- 229920002488 Hemicellulose Polymers 0.000 description 8
- 239000001913 cellulose Substances 0.000 description 7
- 229920002678 cellulose Polymers 0.000 description 7
- 230000000630 rising effect Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- JOOXCMJARBKPKM-UHFFFAOYSA-N 4-oxopentanoic acid Chemical compound CC(=O)CCC(O)=O JOOXCMJARBKPKM-UHFFFAOYSA-N 0.000 description 2
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- -1 hydroxy free radical Chemical class 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000006864 oxidative decomposition reaction Methods 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 150000008163 sugars Chemical class 0.000 description 2
- LWFUFLREGJMOIZ-UHFFFAOYSA-N 3,5-dinitrosalicylic acid Chemical compound OC(=O)C1=CC([N+]([O-])=O)=CC([N+]([O-])=O)=C1O LWFUFLREGJMOIZ-UHFFFAOYSA-N 0.000 description 1
- 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 1
- NOEGNKMFWQHSLB-UHFFFAOYSA-N 5-hydroxymethylfurfural Chemical compound OCC1=CC=C(C=O)O1 NOEGNKMFWQHSLB-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007071 enzymatic hydrolysis Effects 0.000 description 1
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 1
- 229940088598 enzyme Drugs 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Chemical group CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- RJGBSYZFOCAGQY-UHFFFAOYSA-N hydroxymethylfurfural Natural products COC1=CC=C(C=O)O1 RJGBSYZFOCAGQY-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229940040102 levulinic acid Drugs 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D25/00—Filters formed by clamping together several filtering elements or parts of such elements
- B01D25/12—Filter presses, i.e. of the plate or plate and frame type
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D25/00—Filters formed by clamping together several filtering elements or parts of such elements
- B01D25/003—Filters formed by clamping together several filtering elements or parts of such elements integrally combined with devices for controlling the filtration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D25/00—Filters formed by clamping together several filtering elements or parts of such elements
- B01D25/12—Filter presses, i.e. of the plate or plate and frame type
- B01D25/164—Chamber-plate presses, i.e. the sides of the filtering elements being clamped between two successive filtering plates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D25/00—Filters formed by clamping together several filtering elements or parts of such elements
- B01D25/30—Feeding devices ; Discharge devices
- B01D25/302—Feeding devices ; Discharge devices specially adapted for chamber filter presses
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D25/00—Filters formed by clamping together several filtering elements or parts of such elements
- B01D25/32—Removal of the filter cakes
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/16—Inorganic impregnating agents
- B27K3/20—Compounds of alkali metals or ammonium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/16—Inorganic impregnating agents
- B27K3/22—Compounds of zinc or copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/16—Inorganic impregnating agents
- B27K3/32—Mixtures of different inorganic impregnating agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27L—REMOVING BARK OR VESTIGES OF BRANCHES; SPLITTING WOOD; MANUFACTURE OF VENEER, WOODEN STICKS, WOOD SHAVINGS, WOOD FIBRES OR WOOD POWDER
- B27L11/00—Manufacture of wood shavings, chips, powder, or the like; Tools therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27M—WORKING OF WOOD NOT PROVIDED FOR IN SUBCLASSES B27B - B27L; MANUFACTURE OF SPECIFIC WOODEN ARTICLES
- B27M1/00—Working of wood not provided for in subclasses B27B - B27L, e.g. by stretching
- B27M1/08—Working of wood not provided for in subclasses B27B - B27L, e.g. by stretching by multi-step processes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K2200/00—Wooden materials to be treated
- B27K2200/15—Pretreated particles or fibres
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Forests & Forestry (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a device and a method for separating sugar solution and lignin in a lignin preparation process by an organic solvent method, and belongs to the technical field of sugar solution and lignin separation. The utility model provides a sugar liquid and lignin splitter among organic solvent method lignin preparation process includes the switch board and all with the feed arrangement, washing unit, hydraulic pressure station and the filter-pressing device of switch board electrical signal connection, feed arrangement with washing unit all with filter-pressing device is linked together, filter-pressing device includes frame, hydro-cylinder, pressure strip, thrust plate and a plurality of filter plate subassembly, the hydraulic pressure station with the hydro-cylinder is connected, the hydro-cylinder with the pressure strip transmission is connected, a plurality of filter plate subassembly all sliding fit is in the frame, the thrust plate is located the one end of frame and with filter plate subassembly looks adaptation.
Description
Technical Field
The invention relates to the technical field of separation of sugar solution and lignin, in particular to a device and a method for separating the sugar solution from the lignin in the lignin preparation process by an organic solvent method.
Background
The diaphragm filter press, namely the diaphragm filter press, is a filter press with an elastic membrane between a filter plate and filter cloth. In the use process, when the feeding is finished, high-pressure fluid or gas medium can be injected into the diaphragm plate, and then the whole diaphragm can bulge to press the filter cake, so that further dehydration of the filter cake, namely, the common squeezing filtration, is realized. Before the diaphragm filter press process, sugar liquor and lignin are required to be separated from corn straw as much as possible, and the existing separation such as water preheating treatment has the advantages of low cost, small limitation of catalyst use, sustainability, environmental friendliness and the like. In addition, the hydrothermal pretreatment can directly dissolve hemicellulose into its sugars (xylose), thereby synthesizing by-products having industrial value, such as xylo-oligosaccharides, furfural and 5-hydroxymethylfurfural, levulinic acid, acetic acid and formic acid. In addition, acidic catalysts can be used to promote dissolution of hemicellulose, thereby significantly improving accessibility and enzymatic hydrolysis of cellulose. Among them, inorganic acids such as sulfuric acid, hydrochloric acid, etc. are more acidic than organic acids, which cause serious equipment corrosiveness and are costly.
Disclosure of Invention
The invention aims to provide a device and a method for separating sugar liquor from lignin in a lignin preparation process by an organic solvent method, which can improve the saccharification yield of cellulose components.
The aim of the invention can be achieved by the following technical scheme:
sugar liquid and lignin splitter in organic solvent method lignin preparation process, splitter include the switch board and all with switch board electrical signal connection's feed arrangement, washing unit, hydraulic pressure station and filter-pressing device, feed arrangement with washing unit all with filter-pressing device is linked together, filter-pressing device includes frame, hydro-cylinder, pressure strip, thrust plate and a plurality of filter plate subassembly, the hydraulic pressure station with the hydro-cylinder is connected, the hydro-cylinder with the pressure strip transmission is connected, a plurality of filter plate subassembly all sliding fit is in the frame, the thrust plate is located the one end of frame and with filter plate subassembly looks adaptation.
As a further scheme of the invention, the filter plate assembly comprises a frame, filter cloth, a plurality of filter plates and a plurality of diaphragm plates which are all matched with the frame, wherein the diaphragm plates are arranged between any two adjacent filter plates, a filter chamber is arranged between the filter plates and the diaphragm plates, feeding channels are arranged on the filter plates and the diaphragm plates, and the filter cloth is arranged on the end face of the filter plate far away from the feeding end.
As a further scheme of the invention, the frame is provided with an air inlet channel, and the air inlet channel is communicated with the diaphragm plate.
As a further scheme of the invention, the filter pressing device further comprises a sealing cover, wherein the sealing cover is provided with a compressed air inlet, a liquid outlet, a washing port and a flushing port, and the bottom of the material pressing device is provided with a material falling hopper.
As a further scheme of the invention, the feeding device comprises a feeding pump and a slurry tank communicated with the feeding pump, and the feeding pump is communicated with the filter pressing device.
As a further scheme of the invention, the flushing device comprises a flushing pump and a water storage tank, and the flushing pump is respectively communicated with the water storage tank and the filter pressing device.
The invention discloses a method for separating sugar liquor and lignin in a lignin preparation process by using the separation equipment, which comprises the following steps:
1) The hydraulic station is started, and the oil cylinder drives the compacting plate to move towards the filter plate assembly;
2) The pressing plate drives the filter plate assembly to slide on the frame, and the filter plate assembly is sequentially attached and stopped by the stop plate;
3) The feeding device is used for conveying pretreatment liquid into the filter pressing device, and the pretreatment liquid passes through the filter plate assembly to separate sugar liquid and lignin.
As a further aspect of the present invention, the preparation method of the pretreatment liquid includes the steps of:
s1, drying, crushing and sieving corn stalks to obtain solid particles, adding a mixed solution and a composite catalyst into the solid particles, uniformly stirring, carrying out ultraviolet irradiation treatment, taking solids after solid-liquid separation, and washing and drying to obtain a mixture; wherein the dosage ratio of the solid particles, the mixed solution and the composite catalyst is 3g:100mL:0.08-0.10g; the mixed solution is prepared from hydrogen peroxide, sodium hydroxide and deionized water according to a mass ratio of 2.0-2.2:1: 92-95; the ultraviolet irradiation time is 8-10h; the cleaning condition is that the solid surface is neutral; the drying condition is that the drying is carried out for 6-7 hours at 75-80 ℃;
S2, grinding the mixture, adding sodium citrate solution, carrying out microwave treatment, adding cellulase, uniformly mixing, and stirring for reaction to obtain pretreatment liquid; wherein the grinding condition is that the rotating speed is 500r/min, and the grinding is carried out for 10-15min; the microwave treatment condition is that the microwave treatment is carried out for 2-3min under the microwave power of 200-500W; the dosage ratio of the mixture to the sodium citrate solution is 1-5mg:1mL; the dosage ratio of the mixture to the cellulase is 1g:2.5-2.8FPU; the concentration of the sodium citrate solution is 50mmo l/L, pH and the value is 4.8-5.0; the reaction condition is that stirring reaction is carried out for 48-50h at the temperature of 40-60 ℃ and the rotating speed of 150-250 r/min.
As a further scheme of the invention, the preparation method of the composite catalyst comprises the steps of uniformly mixing sodium borohydride, zinc acetate and titanium dioxide, heating to 500-520 ℃ at a temperature rising rate of 3-5 min/DEG C under an argon atmosphere, preserving heat for 2-2.5h, and cooling to obtain the composite catalyst; wherein, the mass ratio of the sodium borohydride to the titanium dioxide to the zinc acetate is 1:2-2.2:0.4.
The invention has the beneficial effects that:
(1) The invention makes hydrogen peroxide generate more polyhydroxy free radical through ultraviolet irradiation, the hydroxy free radical has strong oxidizing property, and the hydroxy free radical oxidizes lignin and hemicellulose to further depolymerize and dissolve, thereby not only removing lignin, but also leaching hemicellulose, and providing more binding sites for cellulose.
(2) The sodium hydroxide is used for degreasing and saponifying to crack ester and ether bonds in lignin and hemicellulose, so that lignin and some hemicellulose are removed from plant cell walls, the non-productive adsorption of cellulose to lignin is reduced, and enzymes act on cellulose and hemicellulose, so that the utilization efficiency of cellulose to cellulose is improved.
(3) Titanium dioxide is added into a system, can absorb light energy and convert the light energy into electrons and holes, can trigger photolysis, generate a large number of free radicals, further promote the oxidative decomposition of lignin and hemicellulose, sodium chloride can increase the ion concentration in the system, thereby promoting the photodecomposition reaction of garbage, under the action of light, zinc ions are added, the stability of zinc oxide and the electron mobility of titanium dioxide can be enhanced through electron transfer with the titanium dioxide, the absorptivity of light energy is improved, and the active ions are matched with a large number of free radicals to mutually promote the contact with organic matters in the system, thereby promoting the oxidative decomposition of organic matters.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of a device for separating sugar solution from lignin in a lignin production process by an organic solvent method.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art without making creative efforts based on the embodiments of the present invention are included in the protection scope of the present invention.
Sugar liquid and lignin separating equipment in organic solvent method lignin preparation process, separating equipment include the switch board and all with switch board electrical signal connection's feed arrangement 1, washing unit 2, hydraulic pressure station 3 and filter-pressing device 4, feed arrangement 1 with washing unit 2 all with filter-pressing device 4 is linked together, filter-pressing device 4 includes frame 41, hydro-cylinder 42, pressure strip 43, thrust plate 44 and a plurality of filter plate subassembly 45, hydraulic pressure station 3 with hydro-cylinder 42 is connected, hydro-cylinder 42 with pressure strip 43 transmission is connected, a plurality of filter plate subassembly 45 all sliding fit is in on the frame 41, thrust plate 44 locate the one end of frame 41 and with filter plate subassembly 45 looks adaptation.
Wherein, the filter plate assembly 45 includes the frame and all cooperates and locate filter cloth, a plurality of filter plate and a plurality of diaphragm board on the frame, arbitrary adjacent two all be equipped with between the filter plate the diaphragm board, the filter plate with be equipped with the filter chamber between the diaphragm board, a plurality of filter plate and a plurality of all be equipped with the pan feeding passageway on the diaphragm board, the filter cloth is located on the terminal surface that the pan feeding was kept away from to the filter plate. And an air inlet channel is arranged on the frame and communicated with the diaphragm plate. The filter pressing device 4 further comprises a sealing cover, a compressed air inlet, a liquid outlet, a washing port and a flushing port are arranged on the sealing cover, and a blanking hopper is arranged at the bottom of the material pressing device. The feeding device 1 comprises a feeding pump and a slurry tank communicated with the feeding pump, and the feeding pump is communicated with the filter pressing device 4. The flushing device 2 comprises a flushing pump and a water storage tank, and the flushing pump is respectively communicated with the water storage tank and the filter pressing device 4.
The method for separating the sugar solution from the lignin separation equipment in the lignin preparation process by using the separation equipment comprises the following steps:
1) The hydraulic station 3 is started, and the oil cylinder 42 drives the pressing plate 43 to move towards the filter plate assembly 45;
2) The pressing plate 43 drives the filter plate assembly 45 to slide on the frame 41, and the filter plate assembly 45 is sequentially attached and stopped by the check stop of the thrust plate 44;
3) The feeding device 1 conveys the pretreatment liquid into the filter pressing device 4, and the pretreatment liquid is separated into sugar liquid and lignin through the filter plate assembly 45.
Example 1
The preparation method of the pretreatment liquid comprises the following steps:
S1, drying, crushing and sieving corn stalks to obtain solid particles, adding a mixed solution and a composite catalyst into the solid particles, uniformly stirring, carrying out ultraviolet irradiation treatment, taking solids after solid-liquid separation, and washing and drying to obtain a mixture; wherein the dosage ratio of the solid particles, the mixed solution and the composite catalyst is 3g:100mL:0.08g; the mixed solution is prepared from hydrogen peroxide, sodium hydroxide and deionized water according to a mass ratio of 2.0:1: 92; the ultraviolet irradiation time is 8 hours; the cleaning condition is that the solid surface is neutral; the drying condition is that the drying is carried out for 6 hours at 75 ℃;
S2, grinding the mixture, adding sodium citrate solution, carrying out microwave treatment, adding cellulase, uniformly mixing, and stirring for reaction to obtain pretreatment liquid; wherein, the grinding condition is that the rotating speed is 500r/min, and the grinding is carried out for 10min; the microwave treatment condition is that the microwave treatment is carried out for 2min under the microwave power of 200W; the dosage ratio of the mixture to the sodium citrate solution is 1mg:1mL; the dosage ratio of the mixture to the cellulase is 1g:2.5FPU; the concentration of the sodium citrate solution is 50 mmol/L, pH and the value is 4.8; the reaction condition is that stirring reaction is carried out for 48 hours at the temperature of 40 ℃ and the rotating speed of 150 r/min.
The preparation method of the composite catalyst comprises the steps of uniformly mixing sodium borohydride, zinc acetate and titanium dioxide, heating to 500 ℃ at a temperature rising rate of 3 min/DEG C under an argon atmosphere, preserving heat for 2 hours, and cooling to obtain the composite catalyst; wherein, the mass ratio of the sodium borohydride to the titanium dioxide to the zinc acetate is 1:2:0.4.
Example 2
The preparation method of the pretreatment liquid comprises the following steps:
s1, drying, crushing and sieving corn stalks to obtain solid particles, adding a mixed solution and a composite catalyst into the solid particles, uniformly stirring, carrying out ultraviolet irradiation treatment, taking solids after solid-liquid separation, and washing and drying to obtain a mixture; wherein the dosage ratio of the solid particles, the mixed solution and the composite catalyst is 3g:100mL:0.09g; the mixed solution is prepared from hydrogen peroxide, sodium hydroxide and deionized water according to a mass ratio of 2.1:1:93 by mixing; the ultraviolet irradiation time is 9 hours; the cleaning condition is that the solid surface is neutral; the drying condition is that the drying is carried out for 6.5 hours at 78 ℃;
S2, grinding the mixture, adding sodium citrate solution, carrying out microwave treatment, adding cellulase, uniformly mixing, and stirring for reaction to obtain pretreatment liquid; wherein, the grinding condition is that the rotating speed is 500r/min, and the grinding is carried out for 13min; the microwave treatment condition is that the microwave treatment is carried out for 2.5min under the microwave power of 350W; the dosage ratio of the mixture to the sodium citrate solution is 3mg:1mL; the dosage ratio of the mixture to the cellulase is 1g:2.7FPU; the concentration of the sodium citrate solution is 50 mmol/L, pH and the value is 4.9; the reaction condition is that stirring reaction is carried out for 49 hours at the temperature of 50 ℃ and the rotating speed of 180 r/min.
The preparation method of the composite catalyst comprises the steps of uniformly mixing sodium borohydride, zinc acetate and titanium dioxide, heating to 510 ℃ at a temperature rising rate of 4 min/DEG C under an argon atmosphere, preserving heat for 2.2 hours, and cooling to obtain the composite catalyst; wherein, the mass ratio of the sodium borohydride to the titanium dioxide to the zinc acetate is 1:2.1:0.4.
Example 3
The preparation method of the pretreatment liquid comprises the following steps:
S1, drying, crushing and sieving corn stalks to obtain solid particles, adding a mixed solution and a composite catalyst into the solid particles, uniformly stirring, carrying out ultraviolet irradiation treatment, taking solids after solid-liquid separation, and washing and drying to obtain a mixture; wherein the dosage ratio of the solid particles, the mixed solution and the composite catalyst is 3g:100mL:0.10g; the mixed solution is prepared from hydrogen peroxide, sodium hydroxide and deionized water according to a mass ratio of 2.2:1: 95; the ultraviolet irradiation time is 10 hours; the cleaning condition is that the solid surface is neutral; the drying condition is that the drying is carried out for 7 hours at 80 ℃;
S2, grinding the mixture, adding sodium citrate solution, carrying out microwave treatment, adding cellulase, uniformly mixing, and stirring for reaction to obtain pretreatment liquid; wherein, the grinding condition is that the rotating speed is 500r/min, and the grinding is carried out for 15min; the microwave treatment condition is that the microwave treatment is carried out for 2-3min under the microwave power of 200-500W; the dosage ratio of the mixture to the sodium citrate solution is 5mg:1mL; the dosage ratio of the mixture to the cellulase is 1g:2.8FPU; the concentration of the sodium citrate solution is 50 mmol/L, pH and the value is 5.0; the reaction condition is that stirring reaction is carried out for 50 hours at the temperature of 60 ℃ and the rotating speed of 250 r/min.
The preparation method of the composite catalyst comprises the steps of uniformly mixing sodium borohydride, zinc acetate and titanium dioxide, heating to 520 ℃ at a temperature rising rate of 5 min/DEG C under an argon atmosphere, preserving heat for 2.5h, and cooling to obtain the composite catalyst; wherein, the mass ratio of the sodium borohydride to the titanium dioxide to the zinc acetate is 1:2.2:0.4.
Comparative example 1
The difference compared to example 2 is that no hydrogen peroxide is used, the remaining components, preparation steps and parameters are identical.
Comparative example 2
The difference compared to example 2 is that no sodium hydroxide is used, and the remaining components, preparation steps and parameters are identical.
Comparative example 3
The difference compared to example 2 is that no zinc acetate is used, the remaining components, preparation steps and parameters are identical.
Comparative example 4
The difference compared to example 2 is that no titanium dioxide is used, the remaining components, preparation steps and parameters are identical.
Comparative example 5
The difference compared to example 2 is that no complex catalyst is used, the remaining components, preparation steps and parameters are identical.
Comparative example 6
The difference compared to example 2 is that no microwave treatment is performed and the remaining components, preparation steps and parameters are identical.
The amounts of reducing sugars in the pretreatment solutions prepared in examples 1 to 3 and comparative examples 1 to 6 were measured using a 3, 5-dinitrosalicylic acid (DNS) colorimetric method, respectively, and the saccharification rates were calculated by the following formula, and the test results thereof are shown in table 1.
TABLE 1
| Saccharification rate (%) | |
| Example 1 | 91.31 |
| Example 2 | 92.51 |
| Example 3 | 91.95 |
| Comparative example 1 | 81.37 |
| Comparative example 2 | 75.41 |
| Comparative example 3 | 82.33 |
| Comparative example 4 | 72.65 |
| Comparative example 5 | 62.14 |
| Comparative example 6 | 83.79 |
As can be seen from the test results of Table 1, the pretreatment solutions prepared in examples 1 to 3 were significantly higher in saccharification rate than those of comparative examples 1 to 6.
While certain embodiments of the present invention have been described in detail, this disclosure is only for the purpose of illustrating preferred embodiments of the invention and is not to be construed as limiting the scope of the invention. All equivalent changes and modifications within the scope of the present invention are intended to be covered by the present invention.
Claims (8)
1. The method for separating sugar solution from lignin in the lignin preparation process by using an organic solvent method is characterized by comprising the following steps of: the separating equipment comprises a control cabinet, a feeding device (1), a flushing device (2), a hydraulic station (3) and a filter pressing device (4), wherein the feeding device (1), the flushing device (2), the hydraulic station (3) and the filter pressing device (4) are all connected with the control cabinet through electric signals, the filter pressing device (4) comprises a frame (41), an oil cylinder (42), a pressing plate (43), a thrust plate (44) and a plurality of filter plate assemblies (45), the hydraulic station (3) is connected with the oil cylinder (42), the oil cylinder (42) is in transmission connection with the pressing plate (43), the filter plate assemblies (45) are all in sliding fit with the frame (41), and the thrust plate (44) is arranged at one end of the frame (41) and is matched with the filter plate assemblies (45);
the separation method for separating sugar liquor and lignin by using the separation equipment comprises the following steps:
1) the hydraulic station (3) is started, and the oil cylinder (42) drives the compacting plate (43) to move towards the filter plate assembly (45);
2) The compression plate (43) drives the filter plate assembly (45) to slide on the frame (41), and the filter plate assembly (45) is sequentially attached and stopped by the thrust plate (44);
3) The feeding device (1) is used for conveying pretreatment liquid into the filter pressing device (4), and the pretreatment liquid is used for separating sugar liquid and lignin through the filter plate assembly (45);
The preparation method of the pretreatment liquid comprises the following steps:
S1, drying, crushing and sieving corn stalks to obtain solid particles, adding a mixed solution and a composite catalyst into the solid particles, uniformly stirring, carrying out ultraviolet irradiation treatment, taking solids after solid-liquid separation, and washing and drying to obtain a mixture; wherein the mixed solution is prepared from hydrogen peroxide, sodium hydroxide and deionized water according to a mass ratio of 2.0-2.2:1: 92-95;
S2, grinding the mixture, adding sodium citrate solution, carrying out microwave treatment, adding cellulase, uniformly mixing, and stirring for reaction to obtain pretreatment liquid; wherein the microwave treatment condition is that the microwave treatment is carried out for 2-3min under the microwave power of 200-500W;
The preparation method of the composite catalyst comprises the steps of uniformly mixing sodium borohydride, zinc acetate and titanium dioxide, heating to 500-520 ℃ at a heating rate of 3-5 ℃/min under an argon atmosphere, preserving heat for 2-2.5h, and cooling to obtain the composite catalyst.
2. The method for separating sugar solution and lignin in the lignin production process by using an organic solvent method according to claim 1, wherein the filter plate assembly (45) comprises a frame, filter cloth, a plurality of filter plates and a plurality of diaphragm plates which are all matched and arranged on the frame, the diaphragm plates are all arranged between any two adjacent filter plates, a filter chamber is arranged between each filter plate and each diaphragm plate, feeding channels are all arranged on the filter plates and the diaphragm plates, and the filter cloth is arranged on the end face of each filter plate far away from the feeding end.
3. The method for separating sugar solution from lignin in an organic solvent lignin production process according to claim 2, wherein an air inlet channel is provided on the frame, and the air inlet channel is communicated with the diaphragm plate.
4. The method for separating sugar solution from lignin in the lignin production process by using an organic solvent method according to claim 1, wherein the filter pressing device (4) further comprises a sealing cover, a compressed air inlet, a liquid outlet, a washing port and a flushing port are arranged on the sealing cover, and a blanking hopper is arranged at the bottom of the filter pressing device (4).
5. The method for separating sugar solution and lignin in the lignin production process by using an organic solvent method according to claim 1 is characterized in that the feeding device (1) comprises a feeding pump and a slurry pond communicated with the feeding pump, and the feeding pump is communicated with the filter pressing device (4).
6. The method for separating sugar solution and lignin in the lignin production process by using an organic solvent method according to claim 1 is characterized in that the flushing device (2) comprises a flushing pump and a water storage tank, and the flushing pump is respectively communicated with the water storage tank and the filter pressing device (4).
7. The method for separating sugar solution from lignin in the process of preparing lignin by using an organic solvent method according to claim 1, wherein in the step S1, the dosage ratio of the solid particles, the mixed solution and the composite catalyst is 3g:100mL:0.08-0.10g; the ultraviolet irradiation time is 8-10h; the cleaning condition is that the solid surface is neutral; the drying condition is that the drying is carried out for 6-7 hours at 75-80 ℃;
In the step S2, the grinding condition is that the rotating speed is 500r/min, and the grinding is carried out for 10-15min; the dosage ratio of the mixture to the sodium citrate solution is 1-5mg:1mL; the dosage ratio of the mixture to the cellulase is 1g:2.5-2.8FPU; the concentration of the sodium citrate solution is 50mmol/L, pH and the value is 4.8-5.0; the reaction condition is that stirring reaction is carried out for 48-50h at the temperature of 40-60 ℃ and the rotating speed of 150-250 r/min.
8. The method for separating sugar solution from lignin in the lignin preparation process by using an organic solvent method according to claim 1, wherein in the preparation of the composite catalyst, the mass ratio of sodium borohydride to titanium dioxide to zinc acetate is 1:2-2.2:0.4.
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