CN109092212B - Single-bed two-stage continuous operation furfural and paper pulp and lignin poly-generation system and method - Google Patents
Single-bed two-stage continuous operation furfural and paper pulp and lignin poly-generation system and method Download PDFInfo
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- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 title claims abstract description 176
- 229920005610 lignin Polymers 0.000 title claims abstract description 64
- 229920001131 Pulp (paper) Polymers 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000006243 chemical reaction Methods 0.000 claims abstract description 197
- 239000003054 catalyst Substances 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000002904 solvent Substances 0.000 claims abstract description 41
- 230000029087 digestion Effects 0.000 claims abstract description 37
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 239000007789 gas Substances 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000007787 solid Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000009835 boiling Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims description 49
- 238000007599 discharging Methods 0.000 claims description 23
- 239000000047 product Substances 0.000 claims description 22
- 238000000605 extraction Methods 0.000 claims description 17
- 239000003513 alkali Substances 0.000 claims description 12
- 238000001125 extrusion Methods 0.000 claims description 12
- 230000001105 regulatory effect Effects 0.000 claims description 11
- 239000012265 solid product Substances 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 10
- 238000004064 recycling Methods 0.000 claims description 8
- 239000008247 solid mixture Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000005189 flocculation Methods 0.000 claims description 4
- 230000016615 flocculation Effects 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 3
- 239000002841 Lewis acid Substances 0.000 claims description 2
- 230000005484 gravity Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 150000007517 lewis acids Chemical class 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 239000011973 solid acid Substances 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 17
- 230000000694 effects Effects 0.000 abstract description 8
- 238000012546 transfer Methods 0.000 abstract description 7
- 230000006872 improvement Effects 0.000 abstract description 4
- 238000005457 optimization Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 54
- 238000005470 impregnation Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000203 mixture Substances 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 150000002972 pentoses Chemical class 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000010517 secondary reaction Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 3
- 239000003502 gasoline Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 2
- 229940011051 isopropyl acetate Drugs 0.000 description 2
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical group C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
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- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
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- 235000005822 corn Nutrition 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- JESHZQPNPCJVNG-UHFFFAOYSA-L magnesium;sulfite Chemical compound [Mg+2].[O-]S([O-])=O JESHZQPNPCJVNG-UHFFFAOYSA-L 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D45/00—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces
- B01D45/12—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by centrifugal forces
- B01D45/16—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by centrifugal forces generated by the winding course of the gas stream, the centrifugal forces being generated solely or partly by mechanical means, e.g. fixed swirl vanes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
- C07D307/48—Furfural
-
- 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
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/02—Pretreatment of the raw materials by chemical or physical means
- D21B1/021—Pretreatment of the raw materials by chemical or physical means by chemical means
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Catalysts (AREA)
- Furan Compounds (AREA)
Abstract
The invention relates to a single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system and method, wherein the method comprises the steps of mixing and boiling raw materials, steam, a catalyst and a solvent in a pressurized reaction kettle, preparing the furfural, the paper pulp and the lignin simultaneously through reactor structure improvement and parameter optimization, and realizing continuous operation; the internal circulation of the internal cyclone separator, the mixed digestion section and the stripping section, the multiple water vapor distributors and the multiple systems in the pressurized reaction kettle are used circularly, so that the mixing effect of the reaction kettle is improved, the heat and mass transfer and the reaction rate are improved, the material entrainment of a gas outlet of the stripping section is reduced, and the furfural yield and the technical economy of the system are improved; the full mixing of gas, liquid and solid in the reaction kettle and the rapid separation of gas and solid are also beneficial to improving the yield of paper pulp and lignin, thereby achieving the optimal combination of system technology and economy.
Description
Technical Field
The invention relates to a process system and a process method for preparing furfural and poly-generating with paper pulp and lignin.
Background
Furfural, also called 2-furaldehyde, is the most important derivative of furan ring system, has active chemical properties, can prepare a plurality of derivatives through oxidation, condensation and other reactions, and is widely applied to the fields of medicine, plastics, pesticides, oil refining, organic synthesis and preparation of non-petroleum polymers. The synthesis method is divided into a one-step method and a two-step method: the one-step method is that the hydrolysis of pentosan and the dehydration of pentosan to generate furfural are completed in one step in the same hydrolysis reactor, the one-step method has the advantages of low equipment investment and simple operation, and is widely applied in the furfural industry, but the one-step method has the advantages of high steam consumption, low furfural yield and large amount of waste residues, and the method for treating the waste residues at present mainly adopts the coal residue mixed combustion technology to use the furfural waste residues as fuel for generating steam; the two-step method is that pentosan is firstly hydrolyzed at about 100 ℃ to generate pentose, then the pentose is dehydrated and cyclized to generate furfural under the condition of higher temperature, the process of pentose hydrolysis to generate pentose is mature, the condition is mild, the pentose yield reaches more than 95%, but the two-step method is more complex, the equipment investment is high, and the process condition of the second step of dehydration is still immature, so that the method cannot be widely applied to actual industrial production. Biomass contains a large amount of hemicellulose and cellulose, can be subjected to acid hydrolysis to generate furfural or furfural series organic products, and part of furfural and other hydrolysis products dissolved in oil products are dynamically extracted by utilizing gasoline or diesel oil in the hydrolysis process, so that the usable amount of the oil products is indirectly increased, and the aim of producing biological liquid oil products is fulfilled. To date, most of the technologies focus on the preparation of furfural and furfural-series products, lacking in efficient utilization of solid residues and technological solutions for technical and economic overall consideration; a set of device and a technical scheme for efficiently preparing furfural and furfural series products and simultaneously effectively recycling paper pulp and lignin are required to be developed, the mature experience of a one-step method is fully absorbed and obtained through selection of a catalyst and a solvent and optimization of a process route and parameters, the furfural products are prepared in one reactor, the yield of the paper pulp and lignin is maximally improved, and the high-purity furfural products, paper pulp sheets and lignin products can be prepared through further purification, so that the device and the method have huge market potential and commercial prospect.
Disclosure of Invention
The invention aims to solve the problems of single product, large solid waste discharge, serious pollution, poor economy and poor market flexibility of the traditional furfural preparation process, and simultaneously prepares and separates furfural, paper pulp and lignin in one reaction kettle through the selection of a catalyst and a solvent and the improvement of the reaction kettle and the optimization of various process parameters, and develops a set of high-efficiency and energy-saving process device for coproduction of multiple products to simultaneously produce the furfural, the paper pulp and the lignin.
The technical scheme for realizing the purpose of the invention is as follows:
a single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system and method, the system comprises a raw material feeding unit, an impregnating tank, a catalyst solvent feeding unit, a pressurized reaction kettle, a steam inlet unit, a furfural rectifying unit, a liquid-solid product discharging unit, a washing unit, a paper pulp collecting unit and a lignin extracting unit which are sequentially connected in a communicated manner; the method comprises the steps that a pressurizing reaction kettle adopts a steam heating mode, raw materials, a catalyst, a solvent and steam are mixed and reacted in the pressurizing reaction kettle to generate furfural, the pressurizing reaction kettle is kept in a boiling state, solid residues comprise paper pulp and lignin, the upper part of the pressurizing reaction kettle is communicated with a furfural rectifying unit through an air outlet pipe and a connecting pipeline pipe fitting of the reaction kettle, the bottom of the pressurizing reaction kettle is communicated with a discharging tank of a liquid-solid product discharging unit through a plurality of reaction kettle bottom discharging pipes and connecting pipeline pipe fittings of the liquid-solid product discharging unit, the liquid-solid product discharging unit is communicated and connected with a washing unit through pipelines, the washing unit is communicated and connected with a paper pulp collecting unit, and a lignin extracting unit is communicated and connected with a filter of the paper pulp collecting unit.
The single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system and method are characterized in that the raw material feeding unit comprises a lock hopper consisting of a plurality of rotary valves, a screw extrusion feeder and a gas seal system; raw materials are added from a lock hopper, enter a screw extrusion feeder under the action of gravity, a rotary valve and air delivery, and have the functions of conveying, mixing and extruding through the design of screw blades and the coupling adaptation of the screw blades and an outer pipe, and are conveyed to an impregnating tank, and meanwhile, a small amount of inert gas is introduced into the lock hopper to ensure that the pressure of a raw material feeding unit is slightly higher than that of the impregnating tank so as to prevent liquid of the impregnating tank from flowing back to the raw material feeding unit; the combined use of multiple rotary valves, conveying extrusion of screw extrusion feeders and gas seals achieves effective sealing and stable raw material conveyance between the raw material feed unit and the impregnation tank.
According to the single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system and method, the catalyst solvent feeding unit comprises the catalyst solvent mixing equipment and the catalyst solvent feeding pipe which are sequentially communicated and connected, the catalyst solvent feeding pipe is communicated and connected with the impregnating tank, the impregnating tank is communicated and connected with the pressurizing reaction kettle through the horizontal or inclined pipeline, the catalyst, the solvent, the raw materials and the like are mixed in the impregnating tank to pretreat the raw materials, wherein the catalyst comprises various solid acid catalysts, metal or metal oxide catalysts, lewis acid, organic acid and the like, the treatment effect of the pressurizing reaction kettle can be improved, the treatment efficiency can be improved, the residence time of materials in the reaction kettle can be reduced, and the yield of the furfural and the paper pulp can be improved.
According to the single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system and method, a single-bed two-section structure is adopted in the pressurizing reaction kettle, the pressurizing reaction kettle comprises a reaction kettle stripping section with a smaller upper cross-sectional area and a reaction kettle mixed digestion section with a larger lower cross-sectional area, so that the gas speed of the stripping section is improved, the generated furfural is quickly removed, the occurrence of secondary reaction is avoided, the yield of the furfural is improved, an internal cyclone separator is arranged in the reaction kettle stripping section to fully reduce the material entrainment of an air outlet pipe of the reaction kettle, the upper part of the internal cyclone separator is communicated with the air outlet pipe of the reaction kettle, a discharge pipe outlet at the lower part of the cyclone separator is arranged in a low-pressure area at the variable-diameter junction of the reaction kettle stripping section and the reaction kettle mixed digestion section, and a plurality of internal cyclone separators can be arranged in the reaction kettle stripping section;
according to the system and the method for continuously operating the furfural, the paper pulp and the lignin in two sections of a single bed, heat required by the pressurizing reaction kettle is provided by water vapor, the temperature of the reaction kettle is controlled and regulated by the flow of the water vapor, and the flow of an air outlet pipe of the reaction kettle is controlled by the temperature of the reaction kettle, so that the reaction kettle is operated in a boiling state; the reaction kettle mixed digestion section is provided with a first water vapor distributor and a second water vapor distributor which are respectively arranged at the bottom and the upper part of the reaction kettle mixed digestion section, and the reaction kettle mixed digestion section can be also provided with a plurality of water vapor distributors; the pressurizing reaction kettle is also provided with a reaction kettle circulating pipe from the reaction kettle mixing and stewing section to the reaction kettle stripping section, so that the mixed distribution of countercurrent and concurrent flow of gas, liquid and solid is promoted, and the heat and mass transfer and the reaction rate of the system are improved.
The single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system and method are characterized in that the steam inlet unit comprises a steam generation system, a steam inlet pipe and a steam temperature and flow control system, and a steam distributor I and a steam distributor II in the mixed digestion section of the steam inlet pipe and the reaction kettle are connected in a communication way.
The system and the method for coproducing furfural, paper pulp and lignin by continuous operation of a single bed in two sections are characterized in that a furfural rectifying unit comprises a flash tank, an alkali liquor neutralization system and a plurality of rectifying towers, and a pressurizing reaction kettle is communicated with the furfural rectifying unit through a reaction kettle air outlet pipe and a connecting pipe fitting; the catalyst and the solvent recovered by the furfural rectifying unit are returned to the washing unit, the furfural rectifying unit and the washing unit are communicated and connected through a pipeline, and the catalyst and the solvent recovered by the furfural rectifying unit can also be returned to the catalyst solvent feeding unit and the impregnating tank.
According to the system and the method for continuously operating the furfural, the paper pulp and the lignin in two sections of a single bed, the liquid-solid product discharging unit comprises a reaction kettle bottom discharging pipe and a discharging tank, and the pressurizing reaction kettle and the discharging tank are communicated through the reaction kettle bottom discharging pipe and a connecting pipeline pipe fitting.
The single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system and method are characterized in that the washing unit comprises a plurality of acid washing or alkali washing towers and a water washing tower, the liquid-solid product unloading unit is communicated with the washing unit through a pipeline, and the acid washing or alkali washing towers of the washing unit can be input with acid or alkali liquor for acid washing or alkali washing.
The single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system and method are characterized in that the paper pulp collecting unit comprises a filter, a dryer and paper pulp forming equipment which are sequentially connected in a communicated mode, the washing unit is connected with the filter in a communicated mode through a pipeline, solid paper pulp products removed by the filter are conveyed to the dryer, the dryer is connected with the paper pulp forming equipment in a communicated mode, and liquid removed by the filter is conveyed to the lignin extraction unit.
According to the system and the method for continuously operating furfural, paper pulp and lignin poly-generation by using the single-bed two-section method, the lignin extraction unit comprises lignin flocculation sedimentation equipment, lignin filtering equipment and lignin drying equipment which are sequentially connected in a communicated manner, part of waste liquid of the lignin extraction unit is conveyed to the catalyst solvent feeding unit and the impregnating tank, the lignin extraction unit and the catalyst solvent feeding unit are respectively connected with the impregnating tank in a communicated manner through pipelines, and the waste liquid of the lignin extraction unit can be conveyed to the washing unit for recycling.
According to the system and the method for continuously operating the furfural, the paper pulp and the lignin in two sections of a single bed, the extracting solution of the mixed digestion section of the reaction kettle is circularly conveyed to the stripping section and the impregnating tank of the reaction kettle at the upper part by the circulating pipe of the reaction kettle, and the liquid-solid mixture of the impregnating tank enters the position lower than the extracting solution port of the mixed digestion section of the reaction kettle through the feeding pipe of the catalyst solvent and the connecting pipeline.
The single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system and method adopt a single-bed two-section structure, and the pressurizing reaction kettle comprises a stripping section with smaller cross-sectional area on the upper surface and a mixed digestion section with larger cross-sectional area on the lower surface so as to improve the gas speed of the stripping section and quickly remove generated furfural, thereby avoiding secondary reaction to occur so as to improve the yield of the furfural; the catalyst is mixed with the solvent and the raw materials in the impregnation tank to pretreat the raw materials, so that the treatment effect and efficiency of the reaction kettle are improved, the residence time of the materials in the reaction kettle is reduced, and the yields of furfural and paper pulp are improved; the premixed materials enter a mixing and stewing section of a reaction kettle, are mixed with water vapor and react under the action of a catalyst; the sealing of the impregnating tank and the raw material feeding unit is realized by a screw extrusion feeder, a plurality of rotary valves and an air seal to ensure the pressure required by the impregnating tank and the pressurized reaction kettle and prevent the liquid in the impregnating tank from flowing back to the raw material feeding unit, thereby realizing stable and reliable continuous operation; the heat required by the reaction kettle is provided by water vapor, a first water vapor distributor and a second water vapor distributor are arranged at the lower part of the pressurized reaction kettle, the bottom part and the upper part of a mixed digestion section of the reaction kettle are respectively provided, and a plurality of water vapor distributors can be also arranged in the mixed digestion section of the reaction kettle; the reaction kettle is also provided with a reaction kettle circulating pipe from the mixing digestion section to the stripping section, so that the staggered distribution of countercurrent and concurrent flow of gas, liquid and solid is promoted, and the heat and mass transfer and the reaction rate of the system are improved; the extracting solution of the reaction kettle mixed digestion section is circularly conveyed to the reaction kettle stripping section and the impregnating tank at the upper part by the reaction kettle circulating pipe, and the liquid-solid mixture of the impregnating tank enters the position of the lower part of the reaction kettle mixed digestion section lower than the extracting solution port by the catalyst solvent feeding pipe and the connecting pipeline. The temperature of the reaction kettle is controlled and regulated by the flow of steam, and the flow of an air outlet pipe of the reaction kettle is controlled by the temperature of the reaction kettle, so that the reaction kettle is operated in a boiling state; the stripping section of the reaction kettle is provided with an inner cyclone separator to fully reduce material entrainment of an air outlet pipe of the reaction kettle, a gas outlet of the inner cyclone separator is connected with the air outlet pipe of the reaction kettle, and a lower solid discharge port is arranged in a low-pressure area at the junction of the stripping section and the mixed digestion section to reduce the resistance of solid discharge. The gas exhausted from the gas outlet pipe of the reaction kettle enters a furfural rectifying unit to prepare a furfural product, and a part of the collected catalyst and solvent returns to a washing unit for recycling, and can also return to a catalyst solvent feeding unit and an impregnating tank for recycling; the liquid-solid mixture at the bottom of the reaction kettle is conveyed to a discharge tank through a plurality of discharge pipes at the bottom of the reaction kettle, paper pulp is obtained by a filtering unit after acid washing or alkali washing and water washing, and is pressed into a sheet after drying and compression molding; neutralizing, flocculating, settling, filtering and drying filtrate to obtain lignin product; a portion of the liquid discharged from the lignin extraction unit is returned to the catalyst solvent feed unit and the impregnation tank or wash unit to increase the overall utilization of water and catalyst and solvent.
The invention has the positive effects that: (1) According to the method or the system, through the selection of the catalyst and the solvent, the improvement of the structure of the reaction kettle, the combined use of internal and external circulation, and the optimization of the process route and various parameters, the furfural, the paper pulp and the lignin are prepared and separated simultaneously in one reaction kettle, and a set of high-efficiency energy-saving process device for coproduction of multiple products is developed to simultaneously produce the furfural, the paper pulp and the lignin; (2) The pressurizing reaction kettle adopts a single-bed two-section structure, and comprises a stripping section with a smaller upper cross-sectional area and a mixed digestion section with a larger lower cross-sectional area, so that the gas speed of the stripping section is improved, the generated furfural is quickly removed, and the occurrence of secondary reaction is avoided so as to improve the furfural yield; (3) The heat required by the reaction kettle is provided by water vapor, a plurality of water vapor distributors are arranged at the lower part of the reaction kettle, and a reaction kettle circulating pipe from the mixed digestion section to the stripping section is arranged at the bottom and the upper part of the mixed digestion section of the reaction kettle respectively, so that the mixed distribution of countercurrent and concurrent flow of gas, liquid and solid and the full mixing of gas, liquid and solid are promoted, and the heat transfer mass transfer and the reaction rate of the system are improved; (4) The temperature of the reaction kettle is controlled and regulated by the flow of water vapor, so that the reaction kettle is operated in a boiling state, and the flow of an air outlet pipe of the reaction kettle is controlled by the temperature of the reaction kettle; (5) The stripping section of the reaction kettle is provided with an inner cyclone separator to fully reduce material entrainment of an air outlet pipe of the reaction kettle, a gas outlet of the inner cyclone separator is connected with the air outlet pipe of the reaction kettle, and a lower solid discharge port is arranged in a low-pressure area at the juncture of the stripping section and the mixed digestion section to reduce the resistance of solid discharge; (6) The sealing of the impregnating tank and the raw material feeding unit is realized by a screw extrusion feeder, a plurality of rotary valves and an air seal to ensure the pressure required by the impregnating tank and the pressurized reaction kettle and prevent the liquid in the impregnating tank from flowing back to the raw material feeding unit, thereby realizing stable and reliable continuous operation; (7) The catalyst, the solvent and the raw materials are mixed in the impregnation tank to pretreat the raw materials, so that the treatment effect of the reaction kettle is improved, the treatment efficiency is improved, the residence time of the materials in the reaction kettle is reduced, and the yield of furfural and paper pulp is improved.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments that are illustrated in the appended drawings, in which:
FIG. 1 is a schematic diagram of a system and structure of the present invention;
FIG. 2 is a schematic diagram of the system according to embodiments 3 and 4 of the present invention
Wherein:
1 a pressurized reaction kettle, 2 a reaction kettle stripping section, 3 a reaction kettle mixed digestion section, 4 a water vapor inlet pipe, 5 a water vapor distributor I, 6 a water vapor distributor II, 7 a catalyst solvent feeding unit, 8 a reaction kettle air outlet pipe, 9 a furfural rectification unit, 10 a reaction kettle air outlet pipe regulating valve, 11 a cyclone separator, 12 a reaction kettle bottom discharging pipe, 13 a raw material feeding unit, 14 a screw extrusion feeder, 15 a catalyst solvent feeding pipe, 16 a dipping tank, 17 a reaction kettle circulating pipe, 18 a discharging tank, 19 a washing unit, 20 a filter, 21 a dryer, 22 a paper pulp forming device, 23 a lignin extraction unit, 24 a water vapor flow regulating valve
Detailed Description
Example 1, see FIG. 1
The embodiment comprises a raw material feeding unit 13, an impregnating tank 16, a catalyst solvent feeding unit 7, a pressurized reaction kettle 1, a steam inlet unit, a furfural rectifying unit 9, a liquid-solid product discharging unit, a washing unit 19, a pulp collecting unit and a lignin extracting unit 23. The pressurizing reaction kettle 1 adopts a single-bed two-section structure and comprises a reaction kettle stripping section 2 with a smaller upper cross-sectional area and a reaction kettle mixing and steaming section 3 with a larger lower cross-sectional area, so that the gas speed of the stripping section 2 is improved, the generated furfural is quickly removed, the occurrence of secondary reaction is avoided, and the furfural yield is improved; corncob, feCl 3 (60 mmol/L), acetic acid (5 wt.%) mixingThe compounds are mixed in the impregnation tank 16 to pretreat the raw materials, thereby improving the treatment effect and efficiency of the reaction kettle, reducing the residence time of the materials in the reaction kettle, and improving the yield of furfural and paper pulp; the premixed materials enter a mixing and stewing section 3 of the reaction kettle, are mixed with water vapor and are added in FeCl 3 And acetic acid, and various reactions occur under the catalysis of acetic acid; the sealing of the impregnation tank 16 and the raw material feeding unit 13 is achieved by the screw extrusion feeder 14, 2 rotary valves and a nitrogen gas seal to ensure the pressure required for the impregnation tank 16 and the pressurized reaction tank 1 and to prevent the liquid inside the impregnation tank 16 from flowing back to the raw material feeding unit 13, thereby achieving a stable and reliable continuous operation; the heat required by the pressurized reaction kettle 1 is provided by water vapor, a first water vapor distributor 5 and a second water vapor distributor 6 are arranged in a reaction kettle mixing and stewing section 3, and a reaction kettle circulating pipe from the mixing and stewing section 3 to a stripping section 2 is respectively arranged at the bottom and the upper part of the reaction kettle mixing and stewing section 3, so that the mixed distribution of countercurrent and concurrent flow of gas, liquid and solid is promoted, and the heat transfer mass transfer and the reaction rate of the system are improved; the extraction liquid of the reaction kettle mixed digestion section 3 is circularly conveyed to the reaction kettle stripping section 2 and the impregnating tank 16 at the upper part by the reaction kettle circulating pipe 17, and the liquid-solid mixture of the impregnating tank 16 enters the position lower than the extraction liquid port of the reaction kettle mixed digestion section 3 through the catalyst solvent feeding pipe 15 and the connecting pipeline. The temperature of the pressurized reaction kettle 1 is controlled and regulated by the flow of steam, so that the pressurized reaction kettle 1 is operated in a boiling state (160-180 ℃), and the flow of an air outlet pipe 8 of the reaction kettle is controlled by the temperature of the pressurized reaction kettle 1; the reaction kettle stripping section 2 is provided with an internal cyclone separator 11 to fully reduce material entrainment of an air outlet pipe of the reaction kettle, a gas outlet of the internal cyclone separator 11 is connected with the air outlet pipe 8 of the reaction kettle, and a lower solid discharge port is arranged in a low-pressure area at the junction of the stripping section 2 and the mixed digestion section 3 to reduce the resistance of solid discharge. The gas discharged from the gas outlet pipe 8 of the reaction kettle enters a furfural rectifying unit 9 to prepare a furfural product, the yield of the furfural is more than 70%, the recovery rate of acetic acid is 0.4 times higher than the yield of the furfural, and part of the recovered gas is collected and stored, and the other part of recovered gas returns to a washing unit for recycling; the liquid-solid mixture at the bottom of the pressurized reaction kettle 1 is conveyed to a discharge tank 18 by 2 discharge pipes 12 at the bottom of the reaction kettle and passes through the second washing unitAfter acid washing (ph=4) and water washing, the pulp is obtained by a filter 20, which is dried by a dryer 21 and pressed into a sheet after press molding treatment by a pulp molding apparatus 22, and pulp yield>90%; delivering the filtrate to a lignin extraction unit 23, adding acetic acid and chitin for flocculation sedimentation, and filtering and drying to obtain lignin products; a part of the liquid discharged from the lignin extraction unit is returned to the catalyst solvent feed unit 15 and the impregnation tank 16 to increase water, feCl 3 And the comprehensive utilization rate of acetic acid.
Example 2, see FIG. 1
The difference between this embodiment and embodiment 1 is that: saw dust, al 2 (SO 4 ) 3 The mixture of acetic acid is mixed in the impregnation tank 16 to pretreat the raw materials, thereby improving the treatment effect and efficiency of the reaction kettle, reducing the residence time of the materials in the reaction kettle and improving the yield of furfural and paper pulp; the premixed materials enter a mixing and stewing section 3 of the reaction kettle, are mixed with water vapor and are mixed with Al 2 (SO 4 ) 3 And acetic acid, and various reactions occur under the catalysis of acetic acid; the other system composition was the same as in example 1.
Example 3, see FIG. 2
The difference between this embodiment and embodiment 1 is that: wheat straw and FeCl 3 The mixture of acetic acid and isopropyl acetate is mixed in the impregnation tank 16 to pretreat the raw materials, thereby improving the treatment effect and efficiency of the reaction kettle, reducing the residence time of the materials in the reaction kettle, and improving the yield of furfural and paper pulp; the premixed materials enter a mixing and stewing section 3 of the reaction kettle, are mixed with water vapor and are added in FeCl 3 And acetic acid, and various reactions occur under the catalysis of acetic acid; the gas discharged from the gas outlet pipe 8 of the reaction kettle enters a furfural rectifying unit 9 to prepare a furfural product, the yield of the furfural is more than 70%, and the collected acetic acid and isopropyl acetate are returned to a catalyst solvent feeding unit and an impregnating tank for recycling; a part of the liquid discharged from the lignin extraction unit is returned to the washing unit 19 to improve the comprehensive utilization rate of water and acetic acid; the other system composition was the same as in example 1.
Example 4, see FIG. 2
Zone of the present example and example 1The other points are as follows: corn stalk and AlCl 3 The mixture of acetic acid and gasoline is mixed in the impregnation tank 16 to pretreat the raw materials, thereby improving the treatment effect and efficiency of the reaction kettle, reducing the residence time of the materials in the reaction kettle and improving the yield of furfural and paper pulp; the premixed materials enter a mixing and stewing section 3 of the reaction kettle, are mixed with water vapor and are mixed in AlCl 3 And acetic acid, and various reactions occur under the catalysis of acetic acid; the gas discharged from the gas outlet pipe 8 of the reaction kettle enters the furfural rectifying unit 9 to prepare a gasoline furfural product, the furfural yield is more than 70%, and part of the collected acetic acid returns to the catalyst solvent feeding unit and the impregnating tank for recycling; the liquid-solid mixture at the bottom of the pressurized reactor 1 is fed from 2 reactor discharge pipes 12 to a discharge tank 18, after alkali washing (0.2M NaOH injection) and water washing in a washing unit, pulp is obtained by a filter 20, which is dried by a dryer 21 and press-molded by a pulp molding apparatus 22, and then pressed into a sheet, the pulp yield>90%; delivering the filtrate to a lignin extraction unit 23, adding NaOH and magnesium sulfite for flocculation and sedimentation to obtain lignin, and washing, filtering and drying to obtain lignin products; a part of the liquid discharged from the lignin extraction unit 23 is returned to the washing unit 19 to improve the comprehensive utilization of water and NaOH; the other system composition was the same as in example 1.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.
Claims (4)
1. A single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system is characterized by comprising a raw material feeding unit (13), an impregnating tank (16), a catalyst solvent feeding unit (7), a pressurizing reaction kettle (1), a steam inlet unit, a furfural rectifying unit (9), a liquid-solid product discharging unit, a washing unit (19), a paper pulp collecting unit and a lignin extracting unit (23), wherein the pressurizing reaction kettle adopts a steam heating mode, raw materials, catalysts, solvents and steam are mixed in the pressurizing reaction kettle (1) to react to generate furfural and keep the pressurizing reaction kettle (1) in a boiling state, solid residues comprise paper pulp and lignin, the upper part of the pressurizing reaction kettle (1) is communicated with the furfural rectifying unit (9) through a reaction kettle air outlet pipe (8) and a connecting pipeline pipe fitting, and the bottom of the pressurizing reaction kettle (1) is communicated with the liquid-solid product discharging unit through a pipeline; the liquid-solid product unloading unit is communicated and connected with the washing unit (19) through a pipeline, the washing unit (19) is communicated and connected with the paper pulp collecting unit through a pipeline, and the lignin extracting unit (23) is communicated and connected with the filter (20) of the paper pulp collecting unit through a pipeline;
the raw material feeding unit (13) comprises a lock hopper consisting of a plurality of rotary valves, a screw extrusion feeder (14) and an air sealing system; raw materials are added from a lock hopper, enter a screw extrusion feeder (14) under the action of gravity and a rotary valve, the screw extrusion feeder (14) conveys the raw materials to an impregnating tank (16), and inert gas is introduced into the lock hopper;
the catalyst solvent feeding unit (7) comprises a catalyst solvent mixing device and a catalyst solvent feeding pipe (15) which are sequentially communicated and connected, the catalyst solvent feeding pipe (15) is communicated and connected with an impregnating tank (16), the impregnating tank (16) is communicated and connected with the pressurized reaction kettle (1) through a horizontal or inclined pipeline, and the catalyst comprises various solid acid catalysts, metal or metal oxide catalysts, lewis acid and organic acid;
the pressurizing reaction kettle (1) adopts a single-bed two-section structure, and comprises a reaction kettle steam stripping section (2) with a smaller upper cross-sectional area and a reaction kettle mixed digestion section (3) with a larger lower cross-sectional area, an internal cyclone separator (11) is arranged in the reaction kettle steam stripping section (2), the upper part of the internal cyclone separator (11) is communicated with a reaction kettle air outlet pipe (8), a discharging pipe outlet at the lower part of the cyclone separator (11) is arranged at the junction of the reaction kettle steam stripping section (2) and the reaction kettle mixed digestion section (3), the reaction kettle mixed digestion section (3) is provided with a water vapor distributor I (5) and a water vapor distributor II (6), and the pressurizing reaction kettle (1) is also provided with a reaction kettle circulating pipe (17) from the reaction kettle mixed digestion section (3) to the reaction kettle steam stripping section (2);
the steam inlet unit comprises a steam generation system, a steam inlet pipe (4) and a steam temperature and flow control system, wherein the steam inlet pipe (4) is communicated with a steam distributor I (5) and a steam distributor II (6) in the reaction kettle mixed digestion section (3);
the furfural rectifying unit (9) comprises a flash tank, an alkali liquor neutralization system and a plurality of rectifying towers, and the pressurizing reaction kettle (1) and the furfural rectifying unit (9) are communicated with a connecting pipeline pipe fitting through a reaction kettle air outlet pipe (8); the catalyst and the solvent recovered by the furfural rectifying unit (9) are returned to the washing unit (19), the furfural rectifying unit (9) and the washing unit (19) are communicated and connected through a pipeline, and the wastewater of the furfural rectifying unit (9) is treated and then used as water vapor, and enters a water vapor inlet unit for recycling;
the liquid-solid product discharging unit comprises a reaction kettle bottom discharging pipe (12) and a discharging tank (18), and the pressurizing reaction kettle (1) and the discharging tank (18) are communicated with the connecting pipe fitting through a plurality of reaction kettle bottom discharging pipes (12);
the washing unit (19) comprises a plurality of acid washing or alkali washing towers and a plurality of water washing towers, the discharging tank (18) is communicated with the washing unit (19) through a pipeline, and the acid washing or alkali washing towers of the washing unit are input with acid or alkali liquor for acid washing or alkali washing;
the pulp collecting unit comprises a filter (20), a dryer (21) and pulp forming equipment (22) which are sequentially connected in a communicated manner, the washing unit (19) and the filter (20) are connected in a communicated manner through a pipeline, solid pulp products removed by the filter (20) are conveyed to the dryer (21), the dryer (21) is connected with the pulp forming equipment (22) in a communicated manner, and liquid removed by the filter (20) is conveyed to the lignin extracting unit (23);
the lignin extraction unit (23) comprises lignin flocculation sedimentation equipment, lignin filtering equipment and lignin drying equipment which are sequentially connected in a communicated manner, wherein the liquid discharged by the lignin extraction unit (23) is conveyed to the catalyst solvent feeding unit (7) and the impregnating tank (16), and the lignin extraction unit (23), the catalyst solvent feeding unit (7) and the impregnating tank (16) are respectively connected in a communicated manner through pipelines;
one path of extracting solution of the reaction kettle mixed digestion section (3) is conveyed back to the reaction kettle stripping section (2) by a reaction kettle circulating pipe (17), and the other path of extracting solution enters the impregnating tank (16) through a connecting pipeline;
the extracting solution of the reaction kettle mixed digestion section (3) is circularly conveyed to the reaction kettle stripping section (2) and the impregnating tank (16) at the upper part by the reaction kettle circulating pipe (17), and the liquid-solid mixture of the impregnating tank (16) enters the position of the lower part of the reaction kettle mixed digestion section (3) lower than the extracting solution port through the catalyst solvent feeding pipe (15) and the connecting pipeline;
the temperature of the pressurized reaction kettle (1) is regulated by the flow of water vapor, the flow of water vapor is controlled by a water vapor flow regulating valve (24), the flow of a reaction kettle air outlet pipe (8) is regulated by a reaction kettle air outlet pipe regulating valve (10), and the reaction kettle air outlet pipe regulating valve (10) is controlled by the temperature of the pressurized reaction kettle (1) so as to ensure that the pressurized reaction kettle (1) is operated in a boiling state.
2. The single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system according to claim 1 is characterized in that a single-bed two-section structure is adopted in a pressurizing reaction kettle (1), the single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system comprises an upper reaction kettle stripping section (2) and a lower reaction kettle mixed digestion section (3), the cross section area of the reaction kettle stripping section (2) is smaller, the cross section area of the reaction kettle mixed digestion section (3) is larger, a first water vapor distributor (5) and a second water vapor distributor (6) are arranged in the reaction kettle mixed digestion section (3), and a reaction kettle circulating pipe (17) is arranged between the reaction kettle mixed digestion section (3) and the reaction kettle stripping section (2).
3. The single-bed two-section continuous operation furfural and paper pulp and lignin poly-generation system according to claim 1 or 2 is characterized in that the reaction kettle stripping section (2) is provided with an internal cyclone separator (11), a gas outlet of the internal cyclone separator (11) is connected with a reaction kettle gas outlet pipe (8), and a lower solid discharge port is arranged at the reducing juncture of the reaction kettle stripping section (2) and the reaction kettle mixed digestion section (3).
4. The single-bed two-stage continuous operation furfural and pulp and lignin poly-generation system according to claim 1 or 2 is characterized in that the raw material feeding unit (13) adopts a feeding and sealing method combining a rotary valve, a lock hopper, a screw extrusion feeder (14) and a gas seal.
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| US20080299628A1 (en) * | 2007-05-31 | 2008-12-04 | Lignol Energy Corporation | Continuous counter-current organosolv processing of lignocellulosic feedstocks |
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| US3660245A (en) * | 1964-05-22 | 1972-05-02 | Ceskoslovenska Akademie Ved | Apparatus for continuous manufacture of furfural and acetic acid |
| CN101326326A (en) * | 2005-12-07 | 2008-12-17 | 凯利·安东尼·O'弗林 | New catalystic reactor method for producing commercial grade pulp, native lignin and single cell protein |
| CN103380247A (en) * | 2011-02-22 | 2013-10-30 | 安德里兹有限公司 | Method and apparatus to produce pulp using pre- hydrolysis and kraft cooking |
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