CN108912072A - Preparation facilities and method and the application of furfural are produced using straw - Google Patents

Preparation facilities and method and the application of furfural are produced using straw Download PDF

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Publication number
CN108912072A
CN108912072A CN201811169315.3A CN201811169315A CN108912072A CN 108912072 A CN108912072 A CN 108912072A CN 201811169315 A CN201811169315 A CN 201811169315A CN 108912072 A CN108912072 A CN 108912072A
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China
Prior art keywords
tower
furfural
reaction
oral area
straw
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CN201811169315.3A
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Chinese (zh)
Inventor
黄建军
袁峰
孙建
王琴
尹秀梅
刘帅
王凯
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FEICHENG JINWEI MACHINERY CO LTD
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FEICHENG JINWEI MACHINERY CO LTD
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Priority to CN201811169315.3A priority Critical patent/CN108912072A/en
Publication of CN108912072A publication Critical patent/CN108912072A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/02Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
    • C07D307/34Heterocyclic 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
    • C07D307/38Heterocyclic 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
    • C07D307/40Radicals substituted by oxygen atoms
    • C07D307/46Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
    • C07D307/48Furfural
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/02Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
    • C07D307/34Heterocyclic 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
    • C07D307/38Heterocyclic 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
    • C07D307/40Radicals substituted by oxygen atoms
    • C07D307/46Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
    • C07D307/48Furfural
    • C07D307/50Preparation from natural products

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Heat Treatment Of Water, Waste Water Or Sewage (AREA)

Abstract

A kind of preparation facilities and method and application for producing furfural using straw, it include with hydrolysis kettle (1) and hydrolysis kettle (1) is for producing furfural device noumenon to what the particle section of straw was hydrolyzed, it is provided for the squeezing machine (3) of isolated hydrolyzate, it is arranged between hydrolysis kettle (1) and squeezing machine (3) and is used to convey the screw conveyor (2) of the straw particle section mixture of hydrolysis, by producing furfural device noumenon, it realizes to the particle section hydrolysis of straw and furfural finished product, pass through screw conveyor (2) and squeezing machine (3), obtain the hydrolyzate containing furfural, therefore realize that straw produces furfural, improve the utility value of straw.

Description

Preparation facilities and method and the application of furfural are produced using straw
Technical field
Type of the present invention is related to a kind of preparation facilities and method and application, especially a kind of to produce furfural using straw Preparation facilities and method and application.
Background technique
Furfural is a kind of excellent selective solvent, and the raw material of the various furfuran compounds of production, is used in casting Adhesive, tetrahydrofuran, organic synthesis, plastics, medicine, chemical anticorrosion etc. all have been widely used, and furfural is not so far not A kind of Organic chemical products that can only be extracted with plant materials such as agricultural wastes using industrial chemicals synthesis, extract furfural Raw material there are many kinds of, theoretically all higher raw materials of hemi-cellulose content, such as corncob, corn stover, sunflower seed shell, cotton Stalk, straw, cotton seed hulls, bagasse, rice husk, broadleaf etc. can extract furfural, but since hydrolysis process has difficulties, existing The raw material that is crushed mostly with feed particulate material or easily of the raw material that uses of furfural production based on, all based on corncob, according to close A few year furfural furfuryl alcohol market big datas will be as a result, corncob supply will reduce 5% or so, while with biomass power generation row The market dosage of the rapid emergence of industry, corncob greatly improves, and the supply of corncob will be more not easy, when corncob is hydrolyzed After processing, the fiber in corncob is destroyed, the available hydrolyzate by way of filtering, when straw is hydrolyzed After processing, the fiber in straw cannot be destroyed, cannot by way of filtering available hydrolyzate, do not have also now Have and a kind of produces the preparation facilities of furfural using straw and method and application mention to realize that straw produces furfural The utility value of high straw.
Based on applicant's technical problem existing in the Disclosure of invention on July 15th, 2018 and background technique, technology Feature and technical effect make application technical solution of the invention.
Summary of the invention
The object of type of the present invention is a kind of preparation facilities that furfural is produced using straw,
The object of type of the present invention is a kind of preparation method that furfural is produced using straw,
The object of type of the present invention is a kind of application of preparation facilities and method that furfural is produced using straw.
In order to overcome the technical drawbacks described above, the purpose of type of the present invention is to provide a kind of system that furfural is produced using straw Standby device and method and application, therefore realize that straw produces furfural, improve the utility value of straw.
In order to achieve the above objectives, type of the present invention adopts the technical scheme that:A kind of preparation dress for producing furfural using stalk It sets, includes with hydrolysis kettle and hydrolysis kettle is for producing furfural device to what the particle section of straw was hydrolyzed Ontology, the squeezing machine for being provided for isolated hydrolyzate are arranged between hydrolysis kettle and squeezing machine and for conveying water The screw conveyor of the straw particle section mixture of solution.
Furfural device noumenon, screw conveyor and squeezing machine are produced due to devising, it is real by producing furfural device noumenon The hydrolysis containing furfural now is obtained by screw conveyor and squeezing machine to the particle section hydrolysis of straw and furfural finished product Liquid, therefore realize that straw produces furfural, improve the utility value of straw.
The present invention devises, producing furfural for main body in the way of being separated in crude fibre containing liquid Device noumenon is coupled to each other for the screw conveyor of conveying and for isolated squeezing machine.
The present invention devises, in the way of realizing that liquid leaches by squeezing action power screw conveyor and squeezing machine with Produce the connection of furfural device noumenon.
The present invention devises, and produces furfural device noumenon and is set as also including accumulator tank, reaction tower, caustic wash tower, fore-running Tower, rectifying column, finished product accumulator tank and condenser.
The present invention devises, the output end oral area of hydrolysis kettle be set as coupling with the input terminal oral area of screw conveyor and The output end oral area of screw conveyor is set as coupling with the input terminal oral area of squeezing machine, and the fluid output port oral area of squeezing machine is set It is set to and couples with the input terminal oral area of accumulator tank and the output end oral area of accumulator tank is set as input terminal oral area with reaction tower Connection, the output end oral area of reaction tower is set as coupling with the input terminal oral area of caustic wash tower and the output end oral area of caustic wash tower is set It is set to and is coupled by condenser with the input terminal oral area of primary distillation tower, the input terminal oral area of primary distillation tower is set as the input with rectifying column The output end oral area of port part connection and rectifying column is set as coupling with the input terminal oral area of finished product accumulator tank.
The present invention devises, and hydrolysis kettle is set as autoclave body, lid, compression bar, relief valve, support rod and heating port and kettle The upper end port of body is set as input port, and the lower end port of autoclave body is set as output port and in the upper end side of autoclave body face It is respectively arranged with relief valve and heating port, the upper end port portion of autoclave body is provided with support rod and compression bar is set as and supports The connection of bar screw-type, lid are arranged in the upper end port of the autoclave body and bottom end of compression bar head and are set as upper end end face with lid The connection of portion's contact, heating port are set as being connected to heating vapour source, and the lower end port portion of autoclave body is set as and helical feed The input terminal oral area of machine couples and autoclave body is set as tower cylindrical body, and lid is provided in round plate body and compression bar is set as Screw thread rhabodoid, support rod are set as L-shaped rhabodoid and the transverse part of support rod are provided with screw thread hole body.
The present invention devises, and the upper end end face portion and spiral shell of screw conveyor is arranged in the input terminal oral area of screw conveyor The lower end surface portion of screw conveyor is arranged in the output end oral area of rotation conveyer, and the center line of screw conveyor is set as and water The center line of solution kettle is in be mutually perpendicular to be distributed.
The present invention devises, and the upper end end face portion of squeezing machine and the liquid of squeezing machine is arranged in the input terminal oral area of squeezing machine The lower end surface portion of squeezing machine is arranged in body output end oral area, and the end of squeezing machine is arranged in the solid output end oral area of squeezing machine Head.
The present invention devises, and squeezing machine is set as by base, spiral deflector roll, dewatering system, speed reducer and motor form Wiping arrangement, spiral deflector roll are set as the blade with Unequal distance and not equal deep helicals and are set as boring with having for blade welding The roll shaft of degree, dewatering system are set as the separate mesh separation rack with straight barrel type steel skeleton and are set as and separate rack spot welding Stainless steel separate mesh, the separating mesh of stainless steel separate mesh be set as circular hole formula and seam grating.
The present invention devises, and hydrolysis kettle, screw conveyor and squeezing machine are set as in integral type distribution and helical feed Machine is arranged between hydrolysis kettle and squeezing machine.
The present invention devises, accumulator tank and finished product accumulator tank is respectively set to oval tank-like body and accumulator tank is set respectively It is set to and is connected to squeezing machine and reaction tower, finished product accumulator tank is set as being connected to rectifying column.
The present invention devises, reaction tower be set as include tower body I, input pipe I, efferent duct I and saturated steam pipe and The upper end side face of tower body I is provided with input pipe I, the top of tower body I is provided with efferent duct I and in the lower end of tower body I Side surface part is provided with saturated steam pipe, input pipe I is set as being connected to by delivery pump with accumulator tank and efferent duct I be set as with Caustic wash tower connection, saturated steam pipe is set as being connected to heating vapour source and tower body I is set as cylindrical tube shape body, in input pipe I and saturated steam pipe on be respectively arranged with shutoff valve.
The present invention devises, and caustic wash tower is set as including tower body II, input pipe II, input pipe III, efferent duct II and alkali Liquid circulating device and the lower end side face of tower body II is provided with input pipe II, is provided in the upper end side face of tower body II defeated Enter pipe III and the top of tower body II is provided with efferent duct II, a port portion of lye circulator is set as and tower body II The connection of lower end side face and another port part of lye circulator be set as coupling with the bottom of tower body II, input pipe II is set as being connected to reaction tower and input pipe III is set as being connected to by delivery pump with lye accumulator tank, and efferent duct II is arranged To be connected to the condenser connecting with primary distillation tower and tower body II is set as cylindrical tube shape body, cut-off is provided on input pipe III Valve and shutoff valve and circulating pump are provided in lye circulator.
The present invention devises, and the input terminal oral area that condenser is set as heat exchanger and condenser is set as and primary distillation tower Heat exchanger output end oral area connection, the output end oral area of condenser be set as and the input terminal oral area of primary distillation tower join It connects.
The present invention devises, and primary distillation tower is set as the tower body of the valve plate with 28 to 30 layers.
The present invention devises, and rectifying column is set as the tower body with sieve plate, float valve and filler and rectifying column internal pressure It is set as being distributed in negative pressure.
The present invention devises, and hydrolysis kettle is set as dividing according to the isolated mode of pressure of solid night with screw conveyor and squeezing machine Cloth and hydrolysis kettle and accumulator tank, reaction tower, caustic wash tower, primary distillation tower, rectifying column, finished product accumulator tank and condenser be set as according to The mode of liquid-purifying is distributed.
The present invention devises, a kind of preparation method for producing furfural using stalk, and step is:To the plant straw of 1-2cm Stalk particle section is set as 194-236kg/m in density3In the state of be hydrolyzed, the straw particle section hydrolyzed Mixture, by applied external force sugared containing 2-5% sulfuric acid liquid and 2-10% in the straw particle section mixture of hydrolysis The hydrolyzate of liquid leaches, and obtains 3-15% chaff by being vaporized processing to the hydrolyzate containing 2-5% sulfuric acid liquid and 2-10% liquid glucose The reaction vapour of aldehyde is reprocessed to obtain furfural finished product to the reaction vapour of 3-15% furfural.
The present invention devises, and step is:
Straw is cut into hay cutter the particle section of 1-2cm, then with baling press the straw pressure of the particle section of 1-2cm It is stored after contracting bundling, after the straw particle section after tying and sulfuric acid liquid will be torn open by the progress nitration mixture processing of nitration mixture machine, then The straw particle section containing sulfuric acid liquid is fitted into autoclave body with belt conveyor, makes the particle section of straw in autoclave body Density be set as 194-236kg/m3, lid is put into the upper end port of autoclave body, rotates compression bar and support rod, compression bar pair Lid applies sealing force, and 0.3-0.5Mpa, 140-160 DEG C of saturated vapor is injected into autoclave body by heating port, It is hydrolyzed in autoclave body, the hydrolysis period is set as 30 minutes to 60 minutes, after the completion of hydrolysis process, opens pressure release Valve carries out pressure release processing after the completion of pressure release processing to autoclave body and starts screw conveyor, the straw particle section of hydrolysis is mixed It closes object to be input in squeezing machine, the separating treatment of liquid and solid is carried out in squeezing machine, the liquid of separating treatment injects savings The solid of tank, separating treatment prepares raw material or the fuel for boiler for levulic acid, obtains containing in accumulator tank There is the hydrolyzate of 2-5% sulfuric acid liquid and 2-10% liquid glucose,
Delivery pump quantitatively injects hydrolyzate in tower body I from input pipe I, and 1.45Mpa, 200 DEG C of superheated steam pass through saturation Steam pipe heats tower body I, and hydrolyzate is vaporized processing, obtains the reaction vapour of 3-15% furfural, the reaction of 3-15% furfural Vapour is entered in caustic wash tower by efferent duct I, and the reaction solution containing 2-5% sulfuric acid of I bottom of tower body is automatic according to tower bottom level condition Discharge,
Reaction vapour is entered in tower body II by input pipe II, and the lye containing 1-10% sodium hydroxide is quantitative by input pipe III It enters in tower body II, lye carries out the reaction vapour after neutralization reaction is neutralized with vapour is reacted, and the reaction vapour after neutralization passes through It is entered in the heat exchanger of primary distillation tower into efferent duct II and enters back into condenser progress condensation process, obtain stoste, stoste Furfural finished product is obtained by the processing of primary distillation tower and rectifying column, furfural finished product enters finished product accumulator tank, and primary distillation tower tower bottom generates Waste water, carry out waste water evaporation section and form superheated steam, superheated steam enters in saturated steam pipe.
The present invention devises, and step is:
One, it after the straw particle section nitration mixture machine nitration mixture after tying being torn open, is fitted into hydrolysis kettle, is being hydrolyzed with belt conveyor 0.3-0.5Mpa, 140-160 DEG C of saturated vapor is passed through in kettle, the hydrolysis period is 30 minutes to 1 hour, after the completion of hydrolysis, is beaten Hydrolysis kettle pressure relief opening string pot pressure release is opened, after the completion of pressure release, starts screw conveyor, pusher to squeezing machine carries out in squeezing machine The separation of liquid, solid after hydrolysis, the liquid after separation enter storage tank, in case subsequent reaction workshop section uses, after separation Solid separately does it and uses, and can carry out the production of levulic acid or enter the burning that boiler carries out furfural dregs,
Two, hydrolyzate, that is, 2-5% sulfuric acid liquid+2-10% liquid glucose after extruding is hydrolyzed, is temporarily stored in storage tank.When to be used, benefit Quantitatively entered with multistage delivery pump from the top of reaction tower, superheated steam, that is, 1.45Mpa, 200 DEG C from the bottom of reaction tower enter, Reaction tower is sieve-plate tower, 30-40 layers, in reaction tower, carries out the dehydration of pentosan, carries out gas-liquid quality, energy is handed over It changes, reaction vapour both 3-15% furfural vapour discharges at the top of reaction tower of generation is reacted, into caustic wash tower;React the anti-of tower bottom The reaction solution foundation automatic outlet of tower bottom level condition of the i.e. 2-5% sulfuric acid of liquid is answered,
Three, the reaction vapour being discharged at the top of reaction tower enters from the bottom gas phase of caustic wash tower, quantitatively enters at the top of caustic wash tower Lye, that is, 1-10% sodium hydroxide, after acid-base neutralization, after reaction vapour enters condenser condensation, into primary distillation tower, in caustic wash tower Bottom is equipped with NaOH solution circulating pump, and lye is recycled, after neutralization requirement is not achieved in concentration of lye, a part of outlet, and one Divide and continues cycling through use.Acid, that is, formic acid, acetic acid in the main removal reaction vapour of the effect of caustic wash tower, using sieve-plate tower Disk, 10-20 layers.After the reaction vapour being discharged at the top of from caustic wash tower is heated to primary distillation tower first, into after the condensation of stoste condenser, into Enter primary distillation tower, carry out fore-running, subtractive process, the furfural finished product met the requirements, the waste water that primary distillation tower tower bottom generates carries out useless The secondary vapour of water evaporation workshop section, generation enters in reaction tower, realizes recycling for waste water.
The present invention devises, it is a kind of using straw produce furfural preparation facilities and method use corn stover system Take the application on furfural.
The technical effects of the invention are that:It is suitable for the hydrolysis process condition of stalk, expands furfural production raw material range, Furfural production cost is reduced, furfural yield is improved, is hydrolyzed using hydrolysis kettle, helical feed, squeezing machine combining form It is small both to have solved straw bulk density for the method for liquid(95-105㎏/m³)The filled raw material of same volume hydrolysis kettle lack equipment The low technical problem of utilization rate, and solve that straw density is low to be easy with steam to bring pipeline and lower road work into hydrolyzer The technical issues of sequence, by reaction tower, caustic wash tower combine in the way of, solve the problems, such as conventional hydrolysis intermittently operated, the present apparatus can For a long time, stablize, continuous operation, and can be unattended, high degree of automation, stalk is not re-used as fuel combustion but as chaff Aldehyde raw materials for production alleviate environmental protection pressure, while solving existing influence crops germination percentage, crop disease when straw-returning Insect pest increase the problems such as, can continuous and steady operation, be suitble to industrialized production, mainly by hydrolysis kettle, helical feed, squeezing machine, The composition such as reaction tower, caustic wash tower and its auxiliary device, heat exchanger, tank and robot control system(RCS), with existing corncob furfural production technology It compares, the technique and device are preferably suitable for the hydrolysis process condition of stalk, expand furfural production raw material range, reduce chaff Aldehyde production cost, improves furfural yield.The method for obtaining hydrolyzate using hydrolysis kettle, helical feed, squeezing machine combining form, Both it is small to have solved straw bulk density(95-105㎏/m³)It is low that the filled raw material of same volume hydrolysis kettle lack utilization rate of equipment and installations Problem, and solve the problems, such as that straw density is low and be easy to bring pipeline and next procedure into steam in hydrolyzer.It utilizes The mode that reaction tower, caustic wash tower combine, solves the problems, such as conventional hydrolysis intermittently operated, and the present apparatus can long-term, stable, continuous fortune Row, and can be unattended, high degree of automation.
In the technical scheme, the type of straw includes corn, wheat, rice, cotton etc., as long as defending rich in more contractings The plant fiber material of sugar, energy hydrolysis furfural, is suitable for furfural production,
Furfural finished product furfural content >=98.5%, moisture≤0.1%, acidity≤0.016mol/L.
In the technical scheme, furfural device noumenon, helical feed are produced containing what liquid was separated in crude fibre Machine and squeezing machine are important technical characteristic, in preparation facilities and method and the technology of the application neck for producing furfural using straw In domain, there is novelty, creativeness and practicability, term in the technical scheme is all can be special in the art Sharp document explains and understands.
Detailed description of the invention
In order to illustrate more clearly of type embodiment of the present invention or technical solution in the prior art, below will to embodiment or Attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is only Some embodiments of type of the present invention, for those of ordinary skill in the art, without creative efforts, also Other drawings may be obtained according to these drawings without any creative labor.
Fig. 1 is the schematic diagram of the preparation facilities that furfural is produced using straw of type of the present invention,
Fig. 2 is the connection relationship diagram of hydrolysis kettle 1, screw conveyor 2 and squeezing machine 3,
Fig. 3 is the right view of Fig. 2,
Fig. 4 is the connection relationship diagram of reaction tower 5 and caustic wash tower 6,
Hydrolysis kettle -1, screw conveyor -2, squeezing machine -3, accumulator tank -4, reaction tower -5, caustic wash tower -6, primary distillation tower -7, rectifying Tower -8, finished product accumulator tank -9, condenser -10, autoclave body -11, lid -12, compression bar -13, relief valve -14, support rod -15 and heating It is port -16, tower body I -51, input pipe I -52, efferent duct I -53 and full, steam pipe -54, tower body II -61, input pipe II -62, defeated Enter pipe III -63, efferent duct II -64, lye circulator -65.
Specific embodiment
According to guidelines for examination, to such as " having ", "comprising" and " comprising " term should be managed used in type of the present invention Solution is not allot the presence or addition of one or more of the other element or combinations thereof.
In the description of type of the present invention, it should be noted that term " center ", "lower", "left", "right", " is erected at "upper" Directly ", the orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, and is only Type of the present invention and simplified description for ease of description, rather than the device or element of indication or suggestion meaning must have specifically Orientation is constructed and operated in a specific orientation, therefore should not be understood as the limitation to type of the present invention.In addition, term " first ", " second ", " third " are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance.
In the description of type of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " connected ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or integrally connect It connects;It can be mechanical connection, be also possible to be electrically connected;It can be directly connected, can also indirectly connected through an intermediary, it can To be the connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood with concrete condition Concrete meaning in type of the present invention.
In addition, as long as technical characteristic involved in invention described below type different embodiments is each other not Constituting conflict can be combined with each other.
Below in conjunction with the attached drawing in type embodiment of the present invention, the technical solution in type embodiment of the present invention is carried out clear Chu is fully described by, it is clear that described embodiment is only type a part of the embodiment of the present invention, rather than whole implementation Example.Based on the embodiment in type of the present invention, those of ordinary skill in the art are obtained without making creative work Every other embodiment, belong to the range of type of the present invention protection.
A kind of preparation facilities for producing furfural using straw, Fig. 1 are one of one embodiment of type of the present invention, knot It closes attached drawing and illustrates the present embodiment, include hydrolysis kettle 1, screw conveyor 2, squeezing machine 3, accumulator tank 4, reaction tower 5, alkali cleaning Tower 6, primary distillation tower 7, rectifying column 8, finished product accumulator tank 9 and condenser 10,
The output end oral area of hydrolysis kettle 1 be set as coupling with the input terminal oral area of screw conveyor 2 and screw conveyor 2 it is defeated Outlet oral area is set as coupling with the input terminal oral area of squeezing machine 3, and the fluid output port oral area of squeezing machine 3 is set as and accumulator tank 4 input terminal oral area couples and the output end oral area of accumulator tank 4 is set as coupling with the input terminal oral area of reaction tower 5, reacts The output end oral area of tower 5 is set as coupling with the input terminal oral area of caustic wash tower 6 and the output end oral area of caustic wash tower 6 is set as logical It crosses condenser 10 to couple with the input terminal oral area of primary distillation tower 7, the input terminal oral area of primary distillation tower 7 is set as the input with rectifying column 8 The output end oral area of port part connection and rectifying column 8 is set as coupling with the input terminal oral area of finished product accumulator tank 9.
In the present embodiment, hydrolysis kettle 1 is set as autoclave body 11, lid 12, compression bar 13, relief valve 14, support rod 15 and adds The upper end port of hot end mouthfuls 16 and autoclave body 11 is set as input port, the lower end port of autoclave body 11 be set as output port and It is respectively arranged with relief valve 14 and heating port 16 in the upper side portion of autoclave body 11, is provided in the upper end port portion of autoclave body 11 Support rod 15 and compression bar 13 are set as coupling with 15 screw-type of support rod, and lid 12 is arranged in the upper end port of autoclave body 11 simultaneously And the bottom end head of compression bar 13 is set as coupling with the upper end end face portion contact of lid 12, heating port 16 is set as steaming with heating Vapour source connection, the lower end port portion of autoclave body 11 is set as coupling with the input terminal oral area of screw conveyor 2 and autoclave body 11 is arranged For tower cylindrical body, lid 12 is provided in round plate body and compression bar 13 is set as screw thread rhabodoid, and support rod 15 is set as L Font rhabodoid and the transverse part of support rod 15 is provided with screw thread hole body.
By hydrolysis kettle 1, the support tie point to screw conveyor 2 is formd, by autoclave body 11, is realized and helical feed The connection of machine 2 realizes the processing of the charging to autoclave body 11 by lid 12, compression bar 13 and support rod 15, by relief valve 14, realizes The heat treatment to autoclave body 11 realized by heating port 16 to the reduced pressure treatment of autoclave body 11.
In the present embodiment, the input terminal oral area of screw conveyor 2 be arranged in screw conveyor 2 upper end end face portion and The lower end surface portion of screw conveyor 2, the center line setting of screw conveyor 2 is arranged in the output end oral area of screw conveyor 2 For with the center line of hydrolysis kettle 1 in being mutually perpendicular to be distributed.
By screw conveyor 2, the support tie point to hydrolysis kettle 1 and squeezing machine 3 is formd, it is real by screw conveyor 2 Show the connection with hydrolysis kettle 1, realizes the connection with squeezing machine 3.
In the present embodiment, the upper end end face portion and squeezing machine 3 of squeezing machine 3 is arranged in the input terminal oral area of squeezing machine 3 Fluid output port oral area the lower end surface portion of squeezing machine 3 is set, the solid output end oral area of squeezing machine 3 is arranged in squeezing machine 3 end.
By squeezing machine 3, foring is realized the support tie point of screw conveyor 2 and accumulator tank 4 by squeezing machine 3 With the connection of screw conveyor 2, the connection with accumulator tank 4 is realized.
In the present embodiment, hydrolysis kettle 1, screw conveyor 2 and squeezing machine 3 are set as in integral type distribution and spiral transferring Machine 2 is sent to be arranged between hydrolysis kettle 1 and squeezing machine 3.
By hydrolysis kettle 1, screw conveyor 2 and squeezing machine 3, the separation of the hydrolyzed liquid of straw is realized.
In the present embodiment, accumulator tank 4 and finished product accumulator tank 9 are respectively set to oval tank-like body and accumulator tank 4 divides It is not set as being connected to squeezing machine 3 and reaction tower 5, finished product accumulator tank 9 is set as being connected to rectifying column 8.
By accumulator tank 4, foring the support tie point to squeezing machine 3 and reaction tower 5 is realized and is squeezed by accumulator tank 4 The connection of dry machine 3, realizes the connection with reaction tower 5, by finished product accumulator tank 9, forms the connection of the support to rectifying column 8 Point realizes the connection with rectifying column 8 by finished product accumulator tank 9.
In the present embodiment, reaction tower 5 is set as including tower body I 51, input pipe I 52, efferent duct I 53 and saturated vapor Pipe 54 and the upper end side face of tower body I 51 is provided with input pipe I 52, is provided with efferent duct I 53 simultaneously at the top of tower body I 51 And the lower end side face of tower body I 51 is provided with saturated steam pipe 54, input pipe I 52 is set as through delivery pump and accumulator tank 4 It is connected to and efferent duct I 53 is set as be connected to caustic wash tower 6, saturated steam pipe 54 is set as and heats vapour source and be connected to and tower Body I 51 is set as cylindrical tube shape body, is respectively arranged with shutoff valve on input pipe I 52 and saturated steam pipe 54.
By reaction tower 5, form the support tie point to accumulator tank 4 and caustic wash tower 6, by input pipe I 52, realize with The connection of accumulator tank 4 realizes the connection with caustic wash tower 6 by efferent duct I 53, by saturated steam pipe 54, realizes to tower body I 51 heat treatment.
In the present embodiment, caustic wash tower 6 is set as including tower body II 61, input pipe II 62, input pipe III 63, efferent duct II 64 and lye circulator 65 and the lower end side face of tower body II 61 is provided with input pipe II 62, in the upper of tower body II 61 End side face is provided with input pipe III 63 and the top of tower body II 61 is provided with efferent duct II 64, lye circulator 65 A port portion is set as coupling with the lower end side face of tower body II 61 and another port part of lye circulator 65 is set It is set to and couples with the bottom of tower body II 61, input pipe II 62 is set as being connected to reaction tower 5 and input pipe III 63 is set as logical Delivery pump is crossed to be connected to lye accumulator tank, efferent duct II 64 be set as with and primary distillation tower 7 connect condenser connection and tower body II 61 are set as cylindrical tube shape body, and shutoff valve is provided on input pipe III 63 and is provided in lye circulator 65 Shutoff valve and circulating pump.
By caustic wash tower 6, foring is realized the support tie point of reaction tower 5 and caustic wash tower 6 by input pipe II 62 It is realized the lye injection processing to tower body II 61 by input pipe III 63 with the connection of reaction tower 5 and is realized by efferent duct II 64 Connection with primary distillation tower 7 by lye circulator 65 realizes circular treatment of the lye in tower body II 61.
In the present embodiment, the input terminal oral area that condenser 10 is set as heat exchanger and condenser 10 be set as with just The output end oral area connection of the heat exchanger of tower 7 is evaporated, the output end oral area of condenser 10 is set as the input terminal with primary distillation tower 7 Oral area connection.
By condenser 10, the support tie point to primary distillation tower 7 is formd, by condenser 10, is realized and primary distillation tower 7 Connection realizes the liquefaction processing to the reaction vapour after neutralization.
In the present embodiment, hydrolysis kettle 1 and screw conveyor 2 and squeezing machine 3 are set as according to the isolated side of pressure of solid night Formula distribution and hydrolysis kettle 1 and accumulator tank 4, reaction tower 5, caustic wash tower 6, primary distillation tower 7, rectifying column 8, finished product accumulator tank 9 and condensation Device 10 is set as being distributed in the way of liquid-purifying.
The two of one embodiment of type of the present invention,
In the present embodiment, squeezing machine 3 is set as extracting by base, spiral deflector roll, dewatering system, speed reducer and motor form Device, spiral deflector roll is set as having the blade of Unequal distance and not equal deep helicals and be set as welding with blade has taper Roll shaft, dewatering system are set as the separate mesh separation rack with straight barrel type steel skeleton and are set as and separate rack spot welding not Become rusty steel separate mesh, and the separating mesh of stainless steel separate mesh is set as circular hole formula and seam grating.
By spiral deflector roll and dewatering system, the filtering to liquid in material is realized.
In the present embodiment, primary distillation tower 7 is set as the tower body of the valve plate with 28 to 30 layers.
By primary distillation tower 7, form the support tie point to condenser 10 and rectifying column 8, by condenser 10, realize with The connection of condenser 10, realizes the connection with rectifying column 8, and technical purpose is:The most of moisture in stoste is removed, together When remove a small amount of acetic acid, tower top steams constant boiling mixture, after cooling natural layering, and water layer passes back into tower, and the extraction of aldehyde layer enters Refinement.
In the present embodiment, rectifying column 8 is set as the tower body with sieve plate, float valve and filler and presses inside rectifying column 8 Power is set as being distributed in negative pressure.
By rectifying column 8, foring is realized the support tie point of primary distillation tower 7 and finished product accumulator tank 9 by rectifying column 8 With the connection of primary distillation tower 7, the connection with finished product accumulator tank 9 is realized, technical purpose is:Remove a small amount of water and micro miscellaneous Matter forms the furfural of high-purity.
Second embodiment of type of the present invention, for main body in the way of being separated in crude fibre containing liquid Produce furfural device noumenon, be coupled to each other for the screw conveyor 2 of conveying and for isolated squeezing machine 3.
In the present embodiment, screw conveyor 2 and squeezing machine 3 in the way of realizing that liquid leaches by squeezing action power Couple with furfural device noumenon is produced.
In the present embodiment, producing furfural device noumenon and being set as also includes accumulator tank 4, reaction tower 5, caustic wash tower 6, just Evaporate tower 7, rectifying column 8, finished product accumulator tank 9 and condenser 10.
Second embodiment of type of the present invention be based on one embodiment,
Below with reference to embodiment, the present invention is further described, following embodiment is intended to illustrate invention rather than to the present invention Further limit.
A kind of preparation method for producing furfural using straw, one of one embodiment of type of the present invention, step It is:
Straw is cut into hay cutter the particle section of 1-2cm, then with baling press the straw pressure of the particle section of 1-2cm It is stored after contracting bundling, after the straw particle section after tying and sulfuric acid liquid will be torn open by the progress nitration mixture processing of nitration mixture machine, then The straw particle section containing sulfuric acid liquid is fitted into autoclave body 11 with belt conveyor, makes the particle section of straw in autoclave body Density in 11 is set as 194-236kg/m3, lid 12 is put into the upper end port of autoclave body 11, makes compression bar 13 and support rod 15 Rotation, compression bar 13 to lid 12 apply sealing force, by heating port 16 0.3-0.5Mpa, 140-160 DEG C satisfy It being injected into autoclave body 11 with steam, is hydrolyzed in autoclave body 11, the hydrolysis period is set as 30 minutes to 60 minutes, After the completion of hydrolysis process, relief valve 14 is opened, pressure release processing is carried out after the completion of pressure release processing to autoclave body 11 and starts helical feed The straw particle section mixture of hydrolysis is input in squeezing machine 3 by machine 2, and point of liquid and solid is carried out in squeezing machine 3 From processing, the liquid of separating treatment injects accumulator tank 4, and the solid of separating treatment prepares raw material or be used for for levulic acid The fuel of boiler obtains the hydrolyzate containing 2-5% sulfuric acid liquid and 2-10% liquid glucose in accumulator tank 4,
Delivery pump quantitatively injects hydrolyzate in tower body I 51 from input pipe I 52, and 1.45Mpa, 200 DEG C of superheated steam pass through Saturated steam pipe 54 heats tower body I 51, and hydrolyzate is vaporized processing, obtains the reaction vapour of 3-15% furfural, 3-15% chaff The reaction vapour of aldehyde is entered in caustic wash tower 6 by efferent duct I 53, and the reaction solution containing 2-5% sulfuric acid of I 51 bottom of tower body is according to tower Bottom level condition is automatically drained out,
Reaction vapour is entered in tower body II 61 by input pipe II 62, and the lye containing 1-10% sodium hydroxide passes through input pipe III 63 quantitatively enter in tower body II 61, and lye carries out the reaction vapour after neutralization reaction is neutralized with vapour is reacted, anti-after neutralization It answers vapour to be entered in the heat exchanger of primary distillation tower 7 by entering efferent duct II 64 and enters back into the progress condensation process of condenser 10, Stoste is obtained, stoste obtains furfural finished product by the processing of primary distillation tower 7 and rectifying column 8, and furfural finished product enters finished product accumulator tank 9, the waste water that 7 tower bottom of primary distillation tower generates carries out waste water evaporation section and forms superheated steam, and superheated steam enters saturated steam pipe 54 In.
The two of one embodiment of type of the present invention, step are:
Straw is cut into the particle section of 1cm with hay cutter, then the straw compression of the particle section of 1cm is beaten with baling press It is stored after bundle, after the straw particle section after tying and sulfuric acid liquid will be torn open by the progress nitration mixture processing of nitration mixture machine, then uses skin The straw particle section containing sulfuric acid liquid is fitted into autoclave body 11 with conveyer, makes the particle section of straw in autoclave body 11 Density be set as 194kg/m3, lid 12 is put into the upper end port of autoclave body 11, rotates compression bar 13 and support rod 15, pressure Bar 13 applies sealing force to lid 12, and 0.3Mpa, 140 DEG C of saturated vapor are injected into autoclave body 11 by heating port 16 In, it being hydrolyzed in autoclave body 11, the hydrolysis period is set as 30 minutes, after the completion of hydrolysis process, relief valve 14 is opened, Pressure release processing is carried out after the completion of pressure release processing to autoclave body 11 to start screw conveyor 2, the straw particle section of hydrolysis is mixed It closes object to be input in squeezing machine 3, the separating treatment of liquid and solid is carried out in squeezing machine 3, the liquid of separating treatment injects storage Store tank 4, the solid of separating treatment is used for the fuel of boiler, obtain in accumulator tank 4 containing 2% sulfuric acid liquid and 2% liquid glucose Hydrolyzate,
Delivery pump quantitatively injects hydrolyzate in tower body I 51 from input pipe I 52, and 1.45Mpa, 200 DEG C of superheated steam pass through Saturated steam pipe 54 heats tower body I 51, and hydrolyzate is vaporized processing, obtains the reaction vapour of 3% furfural, 3% furfural it is anti- Vapour is answered to enter in caustic wash tower 6 by efferent duct I 53, the reaction solution containing 2% sulfuric acid of I 51 bottom of tower body is according to tower bottom liquid level feelings Condition is automatically drained out,
Reaction vapour is entered in tower body II 61 by input pipe II 62, and the lye containing 1% sodium hydroxide is fixed by input pipe III 63 Amount enters in tower body II 61, and lye carries out the reaction vapour after neutralization reaction is neutralized with vapour is reacted, the reaction vapour after neutralization Condenser 10 is entered back into heat exchanger by entering primary distillation tower 7 into efferent duct II 64 and carries out condensation process, is obtained Stoste, stoste obtain furfural finished product by the processing of primary distillation tower 7 and rectifying column 8, and furfural finished product enters finished product accumulator tank 9, just The waste water of 7 tower bottom of tower generation is evaporated, waste water evaporation section is carried out and forms superheated steam, superheated steam enters in saturated steam pipe 54.
The three of one embodiment of type of the present invention, step are:
Straw is cut into the particle section of 2cm with hay cutter, then the straw compression of the particle section of 2cm is beaten with baling press It is stored after bundle, after the straw particle section after tying and sulfuric acid liquid will be torn open by the progress nitration mixture processing of nitration mixture machine, then uses skin The straw particle section containing sulfuric acid liquid is fitted into autoclave body 11 with conveyer, makes the particle section of straw in autoclave body 11 Density be set as 236kg/m3, lid 12 is put into the upper end port of autoclave body 11, rotates compression bar 13 and support rod 15, pressure Bar 13 applies sealing force to lid 12, and 0.5Mpa, 160 DEG C of saturated vapor are injected into autoclave body 11 by heating port 16 In, it being hydrolyzed in autoclave body 11, the hydrolysis period is set as 60 minutes, after the completion of hydrolysis process, relief valve 14 is opened, Pressure release processing is carried out after the completion of pressure release processing to autoclave body 11 to start screw conveyor 2, the straw particle section of hydrolysis is mixed It closes object to be input in squeezing machine 3, the separating treatment of liquid and solid is carried out in squeezing machine 3, the liquid of separating treatment injects storage Store tank 4, the solid of separating treatment prepares raw material for levulic acid, obtain in accumulator tank 4 containing 5% sulfuric acid liquid and The hydrolyzate of 10% liquid glucose,
Delivery pump quantitatively injects hydrolyzate in tower body I 51 from input pipe I 52, and 1.45Mpa, 200 DEG C of superheated steam pass through Saturated steam pipe 54 heats tower body I 51, and hydrolyzate is vaporized processing, obtains the reaction vapour of 15% furfural, 15% furfural It reacts vapour to enter in caustic wash tower 6 by efferent duct I 53, the reaction solution containing 5% sulfuric acid of I 51 bottom of tower body is according to tower bottom liquid level Situation is automatically drained out,
Reaction vapour is entered in tower body II 61 by input pipe II 62, and the lye containing 10% sodium hydroxide passes through input pipe III 63 It quantitatively enters in tower body II 61, lye carries out the reaction vapour after neutralization reaction is neutralized with vapour is reacted, the reaction after neutralization Vapour enters back into condenser 10 in the heat exchanger by entering primary distillation tower 7 into efferent duct II 64 and carries out condensation process, obtains To stoste, stoste obtains furfural finished product by the processing of primary distillation tower 7 and rectifying column 8, and furfural finished product enters finished product accumulator tank 9, The waste water that 7 tower bottom of primary distillation tower generates carries out waste water evaporation section and forms superheated steam, and superheated steam enters saturated steam pipe 54 In.
The four of one embodiment of type of the present invention, step are:
Straw is cut into hay cutter the particle section of 1.5cm, then with baling press the straw pressure of the particle section of 1.5cm It is stored after contracting bundling, after the straw particle section after tying and sulfuric acid liquid will be torn open by the progress nitration mixture processing of nitration mixture machine, then The straw particle section containing sulfuric acid liquid is fitted into autoclave body 11 with belt conveyor, makes the particle section of straw in autoclave body Density in 11 is set as 216kg/m3, lid 12 is put into the upper end port of autoclave body 11, rotates compression bar 13 and support rod 15, Compression bar 13 is applied sealing force to lid 12,0.4Mpa, 150 DEG C of saturated vapor are injected by heating port 16 by kettle It in body 11, is hydrolyzed in autoclave body 11, the hydrolysis period is set as 45 minutes, after the completion of hydrolysis process, and opening is let out Pressure valve 14 carries out pressure release processing after the completion of pressure release processing to autoclave body 11 and starts screw conveyor 2, by the straw of hydrolysis Grain section mixture is input in squeezing machine 3, and the separating treatment of liquid and solid, the liquid of separating treatment are carried out in squeezing machine 3 Accumulator tank 4 is injected, the solid of separating treatment prepares raw material or the fuel for boiler for levulic acid, obtains saving The hydrolyzate containing 3.5% sulfuric acid liquid and 6% liquid glucose in tank 4,
Delivery pump quantitatively injects hydrolyzate in tower body I 51 from input pipe I 52, and 1.45Mpa, 200 DEG C of superheated steam pass through Saturated steam pipe 54 heats tower body I 51, and hydrolyzate is vaporized processing, obtains the reaction vapour of 3-15% furfural, 9% furfural It reacts vapour to enter in caustic wash tower 6 by efferent duct I 53, the reaction solution containing 3.5% sulfuric acid of I 51 bottom of tower body is according to tower bottom liquid Position situation is automatically drained out,
Reaction vapour is entered in tower body II 61 by input pipe II 62, and the lye containing 4.5% sodium hydroxide passes through input pipe III 63 It quantitatively enters in tower body II 61, lye carries out the reaction vapour after neutralization reaction is neutralized with vapour is reacted, the reaction after neutralization Vapour enters back into condenser 10 in the heat exchanger by entering primary distillation tower 7 into efferent duct II 64 and carries out condensation process, obtains To stoste, stoste obtains furfural finished product by the processing of primary distillation tower 7 and rectifying column 8, and furfural finished product enters finished product accumulator tank 9, The waste water that 7 tower bottom of primary distillation tower generates carries out waste water evaporation section and forms superheated steam, and superheated steam enters saturated steam pipe 54 In.
The five of one embodiment of type of the present invention, step are:
Its step is:
One, it after the straw particle section nitration mixture machine nitration mixture after tying being torn open, is fitted into hydrolysis kettle, is being hydrolyzed with belt conveyor 0.3-0.5Mpa, 140-160 DEG C of saturated vapor is passed through in kettle, the hydrolysis period is 30 minutes to 1 hour, after the completion of hydrolysis, is beaten Hydrolysis kettle pressure relief opening string pot pressure release is opened, after the completion of pressure release, starts screw conveyor, pusher to squeezing machine carries out in squeezing machine The separation of liquid, solid after hydrolysis, the liquid after separation enter storage tank, in case subsequent reaction workshop section uses, after separation Solid separately does it and uses, and can carry out the production of levulic acid or enter the burning that boiler carries out furfural dregs,
Two, hydrolyzate, that is, 2-5% sulfuric acid liquid+2-10% liquid glucose after extruding is hydrolyzed, is temporarily stored in storage tank, when to be used, benefit Quantitatively entered with multistage delivery pump from the top of reaction tower, superheated steam, that is, 1.45Mpa, 200 DEG C from the bottom of reaction tower enter, Reaction tower is sieve-plate tower, 30-40 layers, in reaction tower, carries out the dehydration of pentosan, carries out gas-liquid quality, energy is handed over It changes, reaction vapour both 3-15% furfural vapour discharges at the top of reaction tower of generation is reacted, into caustic wash tower;React the anti-of tower bottom The reaction solution foundation automatic outlet of tower bottom level condition of the i.e. 2-5% sulfuric acid of liquid is answered,
Three, the reaction vapour being discharged at the top of reaction tower enters from the bottom gas phase of caustic wash tower, quantitatively enters at the top of caustic wash tower Lye, that is, 1-10% sodium hydroxide, after acid-base neutralization, after reaction vapour enters condenser condensation, into primary distillation tower, in caustic wash tower Bottom is equipped with NaOH solution circulating pump, and lye is recycled, after neutralization requirement is not achieved in concentration of lye, a part of outlet, and one Divide and continues cycling through use.Acid, that is, formic acid, acetic acid in the main removal reaction vapour of the effect of caustic wash tower, using sieve-plate tower Disk, 10-20 layers.After the reaction vapour being discharged at the top of from caustic wash tower is heated to primary distillation tower first, into after the condensation of stoste condenser, into Enter primary distillation tower, carry out fore-running, subtractive process, the furfural finished product met the requirements, the waste water that primary distillation tower tower bottom generates carries out useless The secondary vapour of water evaporation workshop section, generation enters in reaction tower, realizes recycling for waste water.
The six of one embodiment of type of the present invention, step are:
Its step is:
One, it after the straw particle section nitration mixture machine nitration mixture after tying being torn open, is fitted into hydrolysis kettle, is being hydrolyzed with belt conveyor The saturated vapor of 0.3Mpa, 140 DEG C are passed through in kettle, the hydrolysis period is 30 minutes, after the completion of hydrolysis, opens hydrolysis kettle pressure relief opening string Pot pressure release, after the completion of pressure release, starts screw conveyor, pusher to squeezing machine, liquid, solid after being hydrolyzed in squeezing machine Separation, the liquid after separation enters storage tank, in case subsequent reaction workshop section uses, the solid after separation separately does its use, can be into The production of row levulic acid enters the burning that boiler carries out furfural dregs,
Two ,+2% liquid glucose of the i.e. 2% sulfuric acid liquid of hydrolyzate after extruding is hydrolyzed, is temporarily stored in storage tank, when to be used, utilizes multistage Delivery pump quantitatively enters from the top of reaction tower, superheated steam, that is, 1.45Mpa, 200 DEG C from the bottom of reaction tower enter, reaction tower For sieve-plate tower, 30 layers, in reaction tower, the dehydration of pentosan is carried out, carries out gas-liquid quality, energy exchange, reaction produces Both 3% furfural vapour is discharged raw reaction vapour at the top of reaction tower, into caustic wash tower;React reaction solution i.e. 2% sulfuric acid of tower bottom Reaction solution according to the automatic outlet of tower bottom level condition,
Three, the reaction vapour being discharged at the top of reaction tower enters from the bottom gas phase of caustic wash tower, quantitatively enters at the top of caustic wash tower Lye i.e. 1% sodium hydroxide, after acid-base neutralization, after reaction vapour enters condenser condensation, into primary distillation tower, at caustic wash tower bottom Portion is equipped with NaOH solution circulating pump, and lye is recycled, after neutralization requirement is not achieved in concentration of lye, a part of outlet, and a part Continue cycling through use, acid, that is, formic acid, acetic acid in the main removal reaction vapour of the effect of caustic wash tower, using sieve tray, 10 layers, after the reaction vapour being discharged from caustic wash tower top is heated to primary distillation tower first, into after the condensation of stoste condenser, into fore-running Tower, carries out fore-running, subtractive process, the furfural finished product met the requirements, and the waste water that primary distillation tower tower bottom generates carries out waste water evaporation The secondary vapour of workshop section, generation enters in reaction tower, realizes recycling for waste water.
The seven of one embodiment of type of the present invention, step are:
Its step is:
One, it after the straw particle section nitration mixture machine nitration mixture after tying being torn open, is fitted into hydrolysis kettle, is being hydrolyzed with belt conveyor The saturated vapor of 0.5Mpa, 160 DEG C are passed through in kettle, the hydrolysis period is 1 hour, after the completion of hydrolysis, opens hydrolysis kettle pressure relief opening string Pot pressure release, after the completion of pressure release, starts screw conveyor, pusher to squeezing machine, liquid, solid after being hydrolyzed in squeezing machine Separation, the liquid after separation enters storage tank, in case subsequent reaction workshop section uses, the solid after separation separately does its use, can be into The production of row levulic acid enters the burning that boiler carries out furfural dregs,
Two ,+10% liquid glucose of the i.e. 5% sulfuric acid liquid of hydrolyzate after extruding is hydrolyzed, is temporarily stored in storage tank, when to be used, using more Grade delivery pump quantitatively enter from the top of reaction tower, superheated steam, that is, 1.45Mpa, 200 DEG C from the bottom of reaction tower enter, reaction Tower is sieve-plate tower, 40 layers, in reaction tower, carries out the dehydration of pentosan, carries out gas-liquid quality, energy exchange, reaction Both 15% furfural vapour is discharged the reaction vapour of generation at the top of reaction tower, into caustic wash tower;React reaction solution i.e. 5% sulphur of tower bottom The reaction solution foundation automatic outlet of tower bottom level condition of acid,
Three, the reaction vapour being discharged at the top of reaction tower enters from the bottom gas phase of caustic wash tower, quantitatively enters at the top of caustic wash tower Lye i.e. 10% sodium hydroxide, after acid-base neutralization, after reaction vapour enters condenser condensation, into primary distillation tower, at caustic wash tower bottom Portion is equipped with NaOH solution circulating pump, and lye is recycled, after neutralization requirement is not achieved in concentration of lye, a part of outlet, and a part Continue cycling through use.Acid, that is, formic acid, acetic acid in the main removal reaction vapour of the effect of caustic wash tower, using sieve tray, 20 layers, after the reaction vapour being discharged from caustic wash tower top is heated to primary distillation tower first, into after the condensation of stoste condenser, into fore-running Tower, carries out fore-running, subtractive process, the furfural finished product met the requirements, and the waste water that primary distillation tower tower bottom generates carries out waste water evaporation The secondary vapour of workshop section, generation enters in reaction tower, realizes recycling for waste water.
The eight of one embodiment of type of the present invention, step are:
Its step is:
One, it after the straw particle section nitration mixture machine nitration mixture after tying being torn open, is fitted into hydrolysis kettle, is being hydrolyzed with belt conveyor The saturated vapor of 0.4Mpa, 150 DEG C are passed through in kettle, the hydrolysis period is 45 minutes, after the completion of hydrolysis, opens hydrolysis kettle pressure relief opening string Pot pressure release, after the completion of pressure release, starts screw conveyor, pusher to squeezing machine, liquid, solid after being hydrolyzed in squeezing machine Separation, the liquid after separation enters storage tank, in case subsequent reaction workshop section uses, the solid after separation separately does its use, can be into The production of row levulic acid enters the burning that boiler carries out furfural dregs,
Two ,+6% liquid glucose of the i.e. 3.5% sulfuric acid liquid of hydrolyzate after extruding is hydrolyzed, is temporarily stored in storage tank.When to be used, using more Grade delivery pump quantitatively enter from the top of reaction tower, superheated steam, that is, 1.45Mpa, 200 DEG C from the bottom of reaction tower enter, reaction Tower is sieve-plate tower, 35 layers, in reaction tower, carries out the dehydration of pentosan, carries out gas-liquid quality, energy exchange, reaction Both 3-15% furfural vapour is discharged the reaction vapour of generation at the top of reaction tower, into caustic wash tower, reacts the reaction solution of tower bottom i.e. The reaction solution foundation automatic outlet of tower bottom level condition of 3.5% sulfuric acid,
Three, the reaction vapour being discharged at the top of reaction tower enters from the bottom gas phase of caustic wash tower, quantitatively enters at the top of caustic wash tower Lye i.e. 5.5% sodium hydroxide, after acid-base neutralization, after reaction vapour enters condenser condensation, into primary distillation tower, in caustic wash tower Bottom is equipped with NaOH solution circulating pump, and lye is recycled, after neutralization requirement is not achieved in concentration of lye, a part of outlet, and one Divide and continues cycling through use.Acid, that is, formic acid, acetic acid in the main removal reaction vapour of the effect of caustic wash tower, using sieve-plate tower Disk, after the reaction vapour being discharged from caustic wash tower top is heated to primary distillation tower first, into after the condensation of stoste condenser, enters by 15 layers Primary distillation tower, carries out fore-running, subtractive process, the furfural finished product met the requirements, and the waste water that primary distillation tower tower bottom generates carries out waste water The secondary vapour of evaporation section, generation enters in reaction tower, realizes recycling for waste water.
In type of the present invention, it is a kind of using straw produce furfural preparation facilities and method use corn stover system Take the application on furfural.
In type of the present invention, straw is crushed using special pulverizer, to the straw particle of 1-2cm Section is set as 194-236kg/m in density3In the state of be hydrolyzed, the mixing of the straw particle section that is hydrolyzed Object, by applied external force in the straw particle section mixture of hydrolysis contain 2-5% sulfuric acid liquid(It can be by being infused in water The mode for entering sulfuric acid dilutes allotment and obtains)With 2-10% liquid glucose(Pentosan)Hydrolyzate leach, by contain 2-5% sulfuric acid Liquid(Allotment can be diluted by way of injecting sulfuric acid in water to obtain)With 2-10% liquid glucose(Pentosan)Hydrolyzate be vaporized Processing obtains the reaction vapour of 3-15% furfural(Contain furfural, water, acids, alcohols, esters, ketone impurity), to 3-15% furfural Reaction vapour is reprocessed to obtain furfural finished product.
When carrying out present invention verifying, furfural is produced using corn stover, obtained furfural preparation rate and yield rate is best, 138-142kg/m is set as in density to the straw particle section of 1-2cm3In the state of be hydrolyzed, hydrolyzed Straw particle section mixture, it is good to straw hydrolysis effect, while can just obtain containing 2-5% in this state The hydrolyzate of sulfuric acid liquid and 2-10% liquid glucose and hydrolysis output of fluid are high, generate applied external force the plant straw of hydrolysis by squeezing machine 3 Being leached containing the hydrolyzate of 2-5% sulfuric acid liquid and 2-10% liquid glucose in stalk particle section mixture, effectively plant straw fibers Separation, improves hydrolyzate leaching efficiency, while the hydrolyzate only containing 2-5% sulfuric acid liquid and 2-10% liquid glucose could pass through vapour Change handles to obtain the reaction vapour of 3-15% furfural, by being vaporized place to the hydrolyzate containing 2-5% sulfuric acid liquid and 2-10% liquid glucose Reason obtains the reaction vapour of 3-15% furfural, is reprocessed to obtain furfural finished product to the reaction vapour of 3-15% furfural, vaporization process obtains Reaction vapour to 3-15% furfural is the best intermediate for producing furfural finished product, and the steam that reaction tower generates adds by caustic wash tower After alkali neutralization, a part of steam enters 7 tower reactor of primary distillation tower, heat is provided to entire rectifying column 8, in fore-running, 7 tower reactor heating processes In, steam temperature declines 20-30 DEG C, and the steam after cooling enters condenser 10 and is condensed into liquid(70-80 DEG C of temperature, aldehyde contenting amount 6-7%), column plate is used into primary distillation tower 7(Bubble-cap or float valve or filler)Gas-liquid separation is carried out, chaff aldehyde is tentatively obtained(Furfural contains Measure 90-92%), rectifying column 8 removes the moisture, the acids that contain in chaff aldehyde(Formic acid, acetic acid), alcohols(Methanol, ethyl alcohol), esters (Ethyl acetate, methyl formate), ketone(Acetone)Equal impurity obtain meeting in Technical furfural GB1926.1-2009 level-one even It is the furfural finished product of top grade standard.
Type of the present invention has the characteristics that lower:
1, furfural device noumenon, screw conveyor 2 and squeezing machine 3 are produced due to devising, it is real by producing furfural device noumenon The water containing furfural now is obtained by screw conveyor 2 and squeezing machine 3 to the particle section hydrolysis of straw and furfural finished product Liquid is solved, therefore realizes that straw produces furfural, improves the utility value of straw.
2, due to devising accumulator tank 4, reaction tower 5, caustic wash tower 6, primary distillation tower 7, rectifying column 8, finished product accumulator tank 9 and condensation Device 10 realizes the purification to furfural.
3, due to devising screw conveyor 2 and squeezing machine 3, the fiber of straw is separated.
4, the restriction of numberical range has been carried out to planform due to devising, has made the technology of numberical range type of the present invention Technical characteristic in scheme is not to be calculated by formula or test the technical characteristic obtained by limited times, experiments have shown that the number The technical characteristic of value range achieves good technical effect.
5, due to devising the technical characteristic of type of the present invention, in the work of the independent and mutual set of technical characteristic With, by experiments have shown that, the performance indexes of type of the present invention is that existing performance indexes is at least 1.7 times, is passed through Assessment has good market value.
There are also others to produce furfural device noumenon, screw conveyor 2 containing what liquid was separated in crude fibre The technical characteristic coupled with squeezing machine 3 is all one of the embodiment of type of the present invention, and each technology of embodiment described above is special Sign can be combined arbitrarily, to meet Patent Law, patent regulation and the requirement of guidelines for examination, no longer to above-mentioned implementation The all possible combined embodiment of each technical characteristic in example is all described.
Above-described embodiment is provided by the present invention to produce the preparation facilities of furfural using straw and method and answer A kind of way of realization, other deformations of provided scheme, increase or reduce composition therein or step according to the present invention Suddenly, other technical fields close with the present invention or by the present invention are used for, are all belonged to the scope of protection of the present invention.

Claims (10)

1. a kind of preparation facilities that furfural is produced using stalk, it is characterized in that:It include with hydrolysis kettle (1) and hydrolysis kettle (1) be used to that the particle section of straw to be hydrolyzed produces furfural device noumenon, is provided for isolated water It solves the squeezing machine (3) of liquid, be arranged between hydrolysis kettle (1) and squeezing machine (3) and for conveying the straw particle hydrolyzed The screw conveyor (2) of section mixture.
2. the preparation facilities according to claim 1 that furfural is produced using stalk, it is characterized in that:According to containing in crude fibre The mode for thering is liquid to be separated for main body produce furfural device noumenon, for conveying screw conveyor (2) and use It is coupled to each other in isolated squeezing machine (3).
3. the preparation facilities according to claim 2 that furfural is produced using stalk, it is characterized in that:According to by squeezing action power The mode for realizing that liquid leaches couples screw conveyor (2) and squeezing machine (3) with furfural device noumenon is produced.
4. the preparation facilities according to claim 1 that furfural is produced using stalk, it is characterized in that:Produce furfural device noumenon It is set as also including accumulator tank (4), reaction tower (5), caustic wash tower (6), primary distillation tower (7), rectifying column (8), finished product accumulator tank (9) With condenser (10).
5. the preparation facilities according to claim 4 that furfural is produced using stalk, it is characterized in that:The output of hydrolysis kettle (1) Port part is set as coupling with the input terminal oral area of screw conveyor (2) and the output end oral area of screw conveyor (2) is arranged To couple with the input terminal oral area of squeezing machine (3), the fluid output port oral area of squeezing machine (3) is set as defeated with accumulator tank (4) The output end oral area of the connection of inbound port portion and accumulator tank (4) is set as coupling with the input terminal oral area of reaction tower (5), reaction tower (5) output end oral area is set as coupling with the input terminal oral area of caustic wash tower (6) and the output end oral area of caustic wash tower (6) is arranged To be coupled by condenser (10) with the input terminal oral area of primary distillation tower (7), the input terminal oral area of primary distillation tower (7) is set as and rectifying The input terminal oral area of tower (8) couples and the output end oral area of rectifying column (8) is set as the input port with finished product accumulator tank (9) Portion's connection.
6. the preparation facilities according to claim 5 that furfural is produced using stalk, it is characterized in that:Hydrolysis kettle (1) is set as Autoclave body (11), lid (12), compression bar (13), relief valve (14), support rod (15) and heating port (16) and autoclave body (11) Upper end port is set as input port, and the lower end port of autoclave body (11) is set as output port and the upper end side in autoclave body (11) Face is respectively arranged with relief valve (14) and heating port (16), and the upper end port portion of autoclave body (11) is provided with support rod (15) And compression bar (13) is set as coupling with support rod (15) screw-type, and lid (12) is arranged in the upper end port of autoclave body (11) simultaneously And compression bar (13) bottom end head be set as couple with the upper end end face portion contact of lid (12), heat port (16) be set as and Heat vapour source connection, the lower end port portion of autoclave body (11) be set as coupling with the input terminal oral area of screw conveyor (2) and Autoclave body (11) is set as tower cylindrical body, lid (12) be provided in round plate body and compression bar (13) to be set as screw thread rod-shaped Body, support rod (15) are set as L-shaped rhabodoid and the transverse part of support rod (15) are provided with screw thread hole body,
Or, upper end end face portion and screw conveyor of the input terminal oral area setting of screw conveyor (2) in screw conveyor (2) (2) output end oral area is arranged in the lower end surface portion of screw conveyor (2), the center line of screw conveyor (2) be set as with The center line of hydrolysis kettle (1) is in be mutually perpendicular to be distributed,
Or, squeezing machine (3) input terminal oral area setting the upper end end face portion of squeezing machine (3) and the liquid of squeezing machine (3) it is defeated The setting of outlet oral area is arranged in the lower end surface portion of squeezing machine (3), the solid output end oral area of squeezing machine (3) in squeezing machine (3) End,
Or, squeezing machine (3) be set as by base, spiral deflector roll, dewatering system, speed reducer and motor form wiping arrangement, spiral shell Rotation deflector roll is set as having Unequal distance and does not wait the blade of deep helicals and be set as the roll shaft with taper welded with blade, takes off Water system is set as the separate mesh separation rack with straight barrel type steel skeleton and is set as dividing with the stainless steel for separating rack spot welding Off-network, the separating mesh of stainless steel separate mesh are set as circular hole formula and seam grating,
Or, hydrolysis kettle (1), screw conveyor (2) and squeezing machine (3) are set as in integral type distribution and screw conveyor (2) It is arranged between hydrolysis kettle (1) and squeezing machine (3),
Or, accumulator tank (4) and finished product accumulator tank (9) are respectively set to oval tank-like body and accumulator tank (4) is respectively set to It being connected to squeezing machine (3) and reaction tower (5), finished product accumulator tank (9) is set as being connected to rectifying column (8),
Or, reaction tower (5) is set as including tower body I (51), input pipe I (52), efferent duct I (53) and saturated steam pipe (54) And the upper end side face of tower body I (51) is provided with input pipe I (52), efferent duct I is provided at the top of tower body I (51) (53) and in the lower end side face of tower body I (51) it is provided with saturated steam pipe (54), input pipe I (52) is set as passing through conveying Pump is connected to and efferent duct I (53) is set as being connected to caustic wash tower (6) with accumulator tank (4), saturated steam pipe (54) be set as and Heating vapour source is connected to and tower body I (51) is set as cylindrical tube shape body, divides on input pipe I (52) and saturated steam pipe (54) It is not provided with shutoff valve,
Or, caustic wash tower (6) is set as including tower body II (61), input pipe II (62), input pipe III (63), efferent duct II (64) It is provided with input pipe II (62) with lye circulator (65) and in the lower end side face of tower body II (61), in tower body II (61) Upper end side face be provided with input pipe III (63) and be provided with efferent duct II (64) at the top of tower body II (61), lye follows The a port portion of loop device (65) is set as coupling with the lower end side face of tower body II (61) and lye circulator (65) Another port part be set as coupling with the bottom of tower body II (61), input pipe II (62) is set as being connected to reaction tower (5) And input pipe III (63) is set as being connected to by delivery pump with lye accumulator tank, and efferent duct II (64) is set as and and primary distillation tower (7) condenser connected is connected to and tower body II (61) is set as cylindrical tube shape body, and cut-off is provided on input pipe III (63) Valve and it is provided with shutoff valve and circulating pump on lye circulator (65),
Or, condenser (10) is set as heat exchanger and the input terminal oral area of condenser (10) is set as and primary distillation tower (7) The output end oral area of heat exchanger couples, and the output end oral area of condenser (10) is set as and the input port of primary distillation tower (7) Portion's connection,
Or, primary distillation tower (7) is set as the tower body of the valve plate with 28 to 30 layers,
Or, rectifying column (8) be set as the tower body with sieve plate, float valve and filler and rectifying column (8) internal pressure be set as be in Negative pressure distribution.
7. the preparation facilities according to claim 5 that furfural is produced using stalk, it is characterized in that:Hydrolysis kettle (1) and spiral Conveyer (2) and squeezing machine (3) be set as forcing according to solid night isolated mode be distributed and hydrolysis kettle (1) and accumulator tank (4), Reaction tower (5), caustic wash tower (6), primary distillation tower (7), rectifying column (8), finished product accumulator tank (9) and condenser (10) are set as according to liquid The mode of body purification is distributed.
8. a kind of preparation method for producing furfural using stalk, step are:Straw is carried out using special pulverizer It crushes, 194-236kg/m is set as in density to the straw particle section of 1-2cm3In the state of be hydrolyzed, obtain The straw particle section mixture of hydrolysis, by applied external force containing in the straw particle section mixture of hydrolysis The hydrolyzate of 2-5% sulfuric acid liquid and 2-10% liquid glucose leaches, by carrying out to containing the hydrolyzate of 2-5% sulfuric acid liquid and 2-10% liquid glucose Vaporization process obtains the reaction vapour of 3-15% furfural, is reprocessed to obtain furfural finished product to the reaction vapour of 3-15% furfural.
9. the preparation method according to claim 8 that furfural is produced using stalk, it is characterized in that:Its step is:
Straw is cut into hay cutter the particle section of 1-2cm, then with baling press the straw pressure of the particle section of 1-2cm It is stored after contracting bundling, after the straw particle section after tying and sulfuric acid liquid will be torn open by the progress nitration mixture processing of nitration mixture machine, then The straw particle section containing sulfuric acid liquid is fitted into autoclave body (11) with belt conveyor, makes the particle section of straw in kettle Density in body (11) is set as 194-236kg/m3, lid (12) is put into the upper end port of autoclave body (11), makes compression bar (13) It is rotated with support rod (15), compression bar (13) is applied sealing force to lid (12), by heating port (16) 0.3- 0.5Mpa, 140-160 DEG C of saturated vapor is injected into autoclave body (11), is hydrolyzed in autoclave body (11), and the period is hydrolyzed It is set as 30 minutes to 60 minutes, after the completion of hydrolysis process, opens relief valve (14), autoclave body (11) are carried out at pressure release Reason starts screw conveyor (2) after the completion of pressure release processing, the straw particle section mixture of hydrolysis is input to squeezing machine (3) in, the separating treatment of liquid and solid is carried out in squeezing machine (3), the liquid of separating treatment injects accumulator tank (4), separation The solid of processing prepares raw material or the fuel for boiler for levulic acid, obtains containing 2- in accumulator tank (4) The hydrolyzate of 5% sulfuric acid liquid and 2-10% liquid glucose,
Delivery pump quantitatively injects hydrolyzate in tower body I (51) from input pipe I (52), 1.45Mpa, 200 DEG C of superheated steam Tower body I (51) is heated by saturated steam pipe (54), hydrolyzate is vaporized processing, the reaction vapour of 3-15% furfural is obtained, The reaction vapour of 3-15% furfural is entered in caustic wash tower (6) by efferent duct I (53), tower body I (51) bottom containing 2-5% sulfuric acid Reaction solution is automatically drained out according to tower bottom level condition,
Reaction vapour is entered in tower body II (61) by input pipe II (62), and the lye containing 1-10% sodium hydroxide passes through input Pipe III (63) quantitatively enters in tower body II (61), and lye carries out the reaction vapour after neutralization reaction is neutralized with vapour is reacted, in Condenser (10) are entered back into heat exchanger of the reaction vapour by entering primary distillation tower (7) into efferent duct II (64) with after Condensation process is carried out, obtains stoste, stoste obtains furfural finished product, furfural finished product by the processing of primary distillation tower (7) and rectifying column (8) It enters finished product accumulator tank (9), the waste water that primary distillation tower (7) tower bottom generates, carries out waste water evaporation section and form superheated steam, overheat Steam enters in saturated steam pipe (54),
Or, its step is:
One, it after the straw particle section nitration mixture machine nitration mixture after tying being torn open, is fitted into hydrolysis kettle, is being hydrolyzed with belt conveyor 0.3-0.5Mpa, 140-160 DEG C of saturated vapor is passed through in kettle, the hydrolysis period is 30 minutes to 1 hour, after the completion of hydrolysis, is beaten Hydrolysis kettle pressure relief opening string pot pressure release is opened, after the completion of pressure release, starts screw conveyor, pusher to squeezing machine carries out in squeezing machine The separation of liquid, solid after hydrolysis, the liquid after separation enter storage tank, in case subsequent reaction workshop section uses, after separation Solid separately does it and uses, and can carry out the production of levulic acid or enter the burning that boiler carries out furfural dregs,
Two, hydrolyzate, that is, 2-5% sulfuric acid liquid+2-10% liquid glucose after extruding is hydrolyzed, is temporarily stored in storage tank, when to be used, benefit Quantitatively entered with multistage delivery pump from the top of reaction tower, superheated steam, that is, 1.45Mpa, 200 DEG C from the bottom of reaction tower enter, Reaction tower is sieve-plate tower, 30-40 layers, in reaction tower, carries out the dehydration of pentosan, carries out gas-liquid quality, energy is handed over It changes, reaction vapour both 3-15% furfural vapour discharges at the top of reaction tower of generation is reacted, into caustic wash tower;React the anti-of tower bottom The reaction solution foundation automatic outlet of tower bottom level condition of the i.e. 2-5% sulfuric acid of liquid is answered,
Three, the reaction vapour being discharged at the top of reaction tower enters from the bottom gas phase of caustic wash tower, quantitatively enters at the top of caustic wash tower Lye, that is, 1-10% sodium hydroxide, after acid-base neutralization, after reaction vapour enters condenser condensation, into primary distillation tower, in caustic wash tower Bottom is equipped with NaOH solution circulating pump, and lye is recycled, after neutralization requirement is not achieved in concentration of lye, a part of outlet, and one Divide and continue cycling through use,
Acid, that is, formic acid, acetic acid in the main removal reaction vapour of the effect of caustic wash tower, using sieve tray, 10-20 layers, from After the reaction vapour being discharged at the top of caustic wash tower is heated to primary distillation tower first, into after the condensation of stoste condenser, into primary distillation tower, carry out Fore-running, subtractive process, the furfural finished product met the requirements, the waste water that primary distillation tower tower bottom generates carry out waste water evaporation section, produce Raw secondary vapour enters in reaction tower, realizes recycling for waste water.
10. a kind of the preparation facilities of furfural is produced using straw and method is producing answering on furfural using corn stover With.
CN201811169315.3A 2018-10-08 2018-10-08 Preparation facilities and method and the application of furfural are produced using straw Pending CN108912072A (en)

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CN110372644A (en) * 2019-08-29 2019-10-25 山东省化工研究院 The nitration mixture method of deoxidation and equipment of biomass material in a kind of furfural production
CN112409306A (en) * 2020-12-10 2021-02-26 汉中市鹏远生物科技有限公司 Hydrolysis method for preparing furfural from wheat straw

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* Cited by examiner, † Cited by third party
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CN110372644A (en) * 2019-08-29 2019-10-25 山东省化工研究院 The nitration mixture method of deoxidation and equipment of biomass material in a kind of furfural production
CN112409306A (en) * 2020-12-10 2021-02-26 汉中市鹏远生物科技有限公司 Hydrolysis method for preparing furfural from wheat straw

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