CN104557813A - Furfural production method - Google Patents
Furfural production method Download PDFInfo
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- CN104557813A CN104557813A CN201410617723.6A CN201410617723A CN104557813A CN 104557813 A CN104557813 A CN 104557813A CN 201410617723 A CN201410617723 A CN 201410617723A CN 104557813 A CN104557813 A CN 104557813A
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- furfural
- reverse osmosis
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- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Furan Compounds (AREA)
Abstract
The invention discloses a furfural production method which comprises the following steps: carrying out filtration and impurity removal by a ceramic membrane to obtain a crude solution; sending the crude solution into a continuous fluid separation device to carry out continuous ion exchange and concentrating the solution out from the continuous fluid separation device through a reverse osmosis system to obtain a concentrated solution; sending the concentrated solution into a hydrolysis system, sending the obtained furfural gas into pre-fractionation and rectification processes to obtain the finished furfural, wherein the pore diameter of the ceramic membrane adopted by ceramic membrane equipment is 5-15 nm; the working conditions of the ceramic membrane are as follows: the temperature is within 32-35 DEG C and the pressure is 0.6-1.0 Mpa; the reverse osmosis membrane adopted during the reverse osmosis concentration is characterized by being a polysulfone and ether sulfone composite reverse osmosis membrane; the working conditions of the reverse osmosis membrane are as follows: the temperature is 30-35 DEG C and the pressure is 2.0-4.0 Mpa. The method is high in yield and high in efficiency.
Description
Technical field
The present invention relates to a kind of production method of furfural.
Background technology
Existing furfural (furfural) has another name called furtural, and be a kind of light yellow or amber crystal clear liquid, mechanical impurity, physical properties: colourless oil liquid, has the special odor of similar phenyl aldehyde.Be exposed to color in light and air and become reddish-brown very soon, inflammable, easy and steam together volatilizees.Its steam and air form explosive mixture, are slightly soluble in water, are soluble in ethanol, ether.Furfural is a kind of important Organic chemical products, and it has purposes widely in fields such as synthetic resins, refining of petroleum, fuel, medicine and light industries.Furfural mainly utilizes the pentosan in plant fiber material to produce, and all plant fiber materials being rich in pentosan are all applicable to furfural production, as corn cob, cotton seed hulls, oil tea shell, Sunflower shell, bagasse and rice husk etc.The main raw material being used as production furan derivatives, is also used as the selective solvent of unsaturated fatty acids compounds of group in separating saturated fatty compounds of group.South China wide geographic area grows cane, and sugarcane is mainly used as sugaring, but its bagasse major part is discarded, causes the waste of resource and the pollution of environment.Also handlebar bagasse is cooked raw material.Papermaking, be difficult to removing because bagasse contains some other materials, the waste liquid that paper-making process is produced not easily processes, and brings new pollution, also have impact on quality and the purposes of paper.
When preparing furfural, plant fiber material is under the effect of an acidic catalyst, and through the pressurization that heats up, pentosan is wherein hydrolyzed and first generates pentose, and then Dehydration obtains furfural.At present, traditional furfural production technology is substantially as follows: plant fiber material is pulverized, mixed acid, hydrolysis, and the furfural gas that hydrolysis produces makes furfural finished product through subsequent handling.Due to the solid impurity containing furfural dregs class in the furfural gas that hydrolysis produces, need to enter subsequent handling again by after the removing of these solid impurities.The solid impurity of current removing furfural gas after hydrolysis kettle, connects cyclone dust removal skim gate remove, also need to increase dust removal installation, and the impurity removal rate of this method is low, at 80% time, which increase distillation load and the cleaning frequency (1 time/20 days) of subsequent processing primary tower, considerably increase the production cost of furfural.
At present, the industrial xylose mother liquid a large amount of with the byproduct in process of corn cob production wood sugar.It is the wood sugar of 50 ~ 55% that crystalline xylose molasses are separated the mother liquor mass content produced, and the arabinose of 18 ~ 20%, the semi-lactosi of 6 ~ 7%, the glucose of 15%, the seminose of 1 ~ 2%, the assorted sugar of 1 ~ 2%, all the other are water.At present, manufacturer cannot extract the wood sugar reclaimed in xylose mother liquid, and directly sold by mother liquor, the financial loss brought is very large.Fine approach that xylose mother liquid utilizes that to take xylose mother liquid as waste furfural be, and there is good economic benefit.
The producing and manufacturing technique of furfural is mainly divided into single stage method and two step method in the world at present.Single stage method is that poly-pentose hydrolysis and dehydration of pentoses generation furfural two-step reaction once complete in same reactor; The main drawback that single stage method exists is that steam consumption is large, furaldehyde yield low (≤55%), produces a large amount of liquid and waste slag produced shortcomings such as grade.Two-step approach is that to be hydrolyzed into process that pentose (wood sugar) and dehydration of pentoses generate furfural be complete at least two different reactors for poly-pentose in raw material; Than single stage method, two-step approach overcomes the difficult problems such as existing furfural production feed stock conversion is low, generation processing wastewater is difficult to improvement, furfural dregs utility value is low.Along with the development of furfurol industry, and the raising of raw material requirements of comprehensive utilization, development two-step approach furfural production technology, the Mierocrystalline cellulose in separate raw materials and hemicellulose are also used respectively, are the inevitable development trend of furfurol industry.But two step method often technical process relative complex, has high input in advance, dewatering process condition is very unripe, popularizes at present and there is many difficulties.
In the prior art, a kind of method of the plant production furfural by process lignocellulose-containing is disclosed in US Patent No. 4971657, its technique is also two-step approach, wherein relating to the production process that pentose is converted into furfural is: the pentose solution obtained in hydrolysis kettle 1 sends into after temperature-pressure in tubular reactor 8 and distillation tower 10 that (plant material is constantly sent in hydrolysis kettle 1 in the process, and be hydrolyzed raw material completely and constantly discharged), pentose generation cyclodehydration reacts, the aldehyde vapour generated enters in collecting tank 14 after over-heat-exchanger 13 condensation, aldehyde liquid in described collecting tank 14 enters into water distilling apparatus 16 after over-heat-exchanger 15 is vaporized, and obtains furfural crude product after distillation, and the waste liquid of discharging from water distilling apparatus 16 returns to hydrolysis kettle 1.Bottom described distillation tower 10 discharge unreacted completely pentose solution in heat exchanger 36 through high pressure steam vaporization after, return in described distillation tower 10, and the waste liquid of discharging from distillation tower 10 end returns hydrolysis kettle by pipeline 11 and heat exchanger 4, different working cycle is realized by by-pass valve control.In technology disclosed in this patent, mainly there is following shortcoming: 1) distillation tower 10 end discharge containing unreacted completely pentose solution by heat exchanger 36 vaporize after again send back in distillation tower 10, do not provide separately dehydration of pentoses reaction unit again, cause pentose transformation efficiency not high; On the other hand, the aldehyde vapour steamed from distillation tower 10 sends into water distilling apparatus 16 after condensation, collection, vaporescence, furfural crude product is obtained through separation, remaining waste liquid returns in hydrolysis kettle 1, but the furfural that may contain in remaining liq is not further separated, but get back to again in hydrolysis system, increase the weight of the burden of whole furfural production system on the one hand, cause the waste of the energy, also the furfural structure generated may be caused on the other hand to be damaged, finally to cause out the reduction of aldehyde rate; 2) pentose is converted into furfural in tubular reactor 8 and distillation tower 10, is converted into the reaction conditions of furfural for reaching pentose, and these two reactors need to provide independent heating and pressurizing equipment respectively, therefore need to consume a large amount of high pressure steam; 3) waste liquid that water distilling apparatus 16 is discharged returns to hydrolyzation system and participates in hydrolysis reaction, but do not disclose the waste water that thick aldehyde treating process produces in patent document and send hydrolysis system back to yet, therefore the waste water that whole furfural production system produces does not obtain whole recycles, does not namely accomplish the complete closed cycle of whole waste water, zero release.
CN1381450A provides a kind of and makes the method for getting furfural from bagasse.Comprise the following steps: that (1) bagasse loads in hydrolyzer after mixing by weight 1: 3 with dilute sulphuric acid (4-10%), with open steam heating, and the furfural generated is taken out of hydrolyzer; (2) containing the vapour condensation (reclaim heat energy and produce secondary steam) of furfural 3-6%, deliver to primary tower distillation, containing furfural about 30% in this overhead condensation liquid, be cooled to 40-50 DEG C of layering; (3) low boilers distillation tower is sent on upper strata, returns primary tower and reclaim furfural after removing low boilers; (4) lower coarse furfural send dehydration tower and treating tower processing, removes the high boiling products such as moisture content, low boilers and methyl furfural respectively, obtains product, lucifuge, deoxygenation, sealed storage.
CN1763024A mono-kind take xylose mother liquid as the method for waste furfural, its feature comprises following process: take xylose mother liquid as raw material, acetic acid, phosphoric acid, sulfuric acid, hydrochloric acid, Sulfated titanium oxide or Sulfated zirconium white are catalyzer, with sodium-chlor, Repone K, zinc chloride, double superhosphate, sodium sulfate, potassium sulfate or sodium-acetate for promotor.And press xylose mother liquid, water, catalyzer, catalyst aid mass ratio for (6 ~ 100): (100 ~ 300): (3 ~ 12): after (0 ~ 100) mixing, load heating in dehydrating kettle, temperature of reaction is 120 ~ 260 DEG C, and reaction pressure is 0.1 ~ 5.0MPa.The vapour phase that reaction generates obtains furfural aqueous solution through condensation, the above-mentioned xylose mother liquid of furfural is obtained again: water: catalyzer: catalyst aid mass ratio is (20 ~ 80): (150 ~ 250): (5 ~ 10): (0 ~ 80) through steaming water, temperature of reaction is 150 ~ 240 DEG C, reaction pressure 0.5 ~ 3.5MPa, catalyzer is acetic acid, sulfuric acid or Sulfated titanium oxide, and promotor is sodium-chlor, sodium sulfate or zinc chloride.
CN101108838A discloses a kind of system of manufacturing furol with pentose solution, and described furfural preparation system comprises dehydration distillation unit and dewatering and recovery unit.Wherein said dehydration distillation unit at least comprises a dehydration reaction distillation tower, described pentose solution is carried out dehydration distillation and obtains furfuryl aldehyde solution; Described dewatering and recovery unit is connected with described dehydration reaction distillation tower, comprise at least one-level dehydration reactor, dewatering further to the waste water containing pentose of discharging at the bottom of described dehydration reaction distillation tower tower and generate furfural steam returns to described dehydration reaction distillation tower.The dehydration reactor that 2-5 level is connected mutually is set in described dewatering and recovery unit.The top of dehydration reactor described in every one-level is at least provided with a pentose solution entrance, an aldehyde vapor outlet, a steam-in, bottom is at least provided with a waste liquid outlet, and the waste liquid outlet of upper level dehydration reactor is connected with aldehyde vapor outlet with the pentose solution entrance of next stage dehydration reactor respectively with steam-in; The pentose solution entrance of described first step dehydration reactor connects at the bottom of described dehydration reaction distillation tower tower, the waste liquid outlet of described last step dehydration reactor is connected to the hydrolysis system that vegetable fibre is hydrolyzed into pentose solution, sends the waste water of described furfural preparation system back to described hydrolysis system.Described dewatering and recovery unit also comprises the heating unit be connected with the steam-in of dehydration reactor described in last step, delivers to dehydration reactor described in every one-level, and finally give described dehydration reaction distillation tower by described furfural steam by up step by step for heat.Be provided with potential difference between described dehydration reaction distillation tower and described first step dehydration reactor, be provided with potential difference between described often adjacent secondary dehydration reactor, described dehydration reaction distillation tower position is the highest, and described last step dehydration reactor position is minimum.The waste liquid outlet of described dehydration reaction distillation tower is higher than the pentose solution entrance of described first step dehydration reactor, and in described often adjacent secondary dehydration reactor, the waste liquid outlet of upper level is higher than the pentose solution entrance of next stage.
Summary of the invention
The object of the invention is to the production method proposing a kind of furfural.
For reaching this object, the present invention by the following technical solutions:
A production method for furfural, is characterized in that: through ceramic membrane filter removal of impurities, obtains thick liquid after slagging-off; Enter continuous fluid tripping device afterwards, carry out continuous ionic exchange, from continuous fluid tripping device, solution out concentrates through reverse osmosis system again, obtains concentrated solution; Concentrated solution is sent into hydrolysis system, the furfural gas obtained sends into fore-running and rectification working process, furfural finished product is obtained after rectifying, wherein ceramic membrane equips the aperture of the ceramic membrane adopted is 5-15nm, its working conditions is: between temperature 32-35 DEG C, pressure 0.6-1.0Mpa, and the feature of the reverse osmosis membrane that reverse osmosis concentration adopts is polysulfones, polyethersulfone, complex reverse osmosis membrane, its working conditions be temperature at 30 ~ 35 DEG C, operating pressure 2.0 ~ 4.0Mpa.
Embodiment
Embodiment 1
A production method for furfural, is characterized in that: through ceramic membrane filter removal of impurities, obtains thick liquid after slagging-off; Enter continuous fluid tripping device afterwards, carry out continuous ionic exchange, from continuous fluid tripping device, solution out concentrates through reverse osmosis system again, obtains concentrated solution; Concentrated solution is sent into hydrolysis system, the furfural gas obtained sends into fore-running and rectification working process, furfural finished product is obtained after rectifying, wherein ceramic membrane equips the aperture of the ceramic membrane adopted is 20nm, its working conditions is: between temperature 30 DEG C, pressure 0.15Mpa, and the feature of the reverse osmosis membrane that reverse osmosis concentration adopts is polysulfones, polyethersulfone, complex reverse osmosis membrane, its working conditions be temperature at 30 ~ 35 DEG C, operating pressure 2.0 ~ 4.0Mpa.
Embodiment 2
A production method for furfural, is characterized in that: through ceramic membrane filter removal of impurities, obtains thick liquid after slagging-off; Enter continuous fluid tripping device afterwards, carry out continuous ionic exchange, from continuous fluid tripping device, solution out concentrates through reverse osmosis system again, obtains concentrated solution; Concentrated solution is sent into hydrolysis system, the furfural gas obtained sends into fore-running and rectification working process, furfural finished product is obtained after rectifying, wherein ceramic membrane equips the aperture of the ceramic membrane adopted is 50nm, its working conditions is: between temperature 38 DEG C, pressure 0.5Mpa, and the feature of the reverse osmosis membrane that reverse osmosis concentration adopts is polysulfones, polyethersulfone, complex reverse osmosis membrane, its working conditions be temperature at 30 ~ 35 DEG C, operating pressure 2.0 ~ 4.0Mpa.
Embodiment 3
A kind of mechanical workout lapping liquid, containing abrasive material 20, distilled water 80, furfural 0.01, sequestrant 20, oxygenant 10, is weight part.
Embodiment 4
The production method of embodiment 3 furfural used, is characterized in that: through ceramic membrane filter removal of impurities, obtains thick liquid after slagging-off; Enter continuous fluid tripping device afterwards, carry out continuous ionic exchange, from continuous fluid tripping device, solution out concentrates through reverse osmosis system again, obtains concentrated solution; Concentrated solution is sent into hydrolysis system, the furfural gas obtained sends into fore-running and rectification working process, furfural finished product is obtained after rectifying, wherein ceramic membrane equips the aperture of the ceramic membrane adopted is 5-15nm, its working conditions is: between temperature 32-35 DEG C, pressure 0.6-1.0Mpa, and the feature of the reverse osmosis membrane that reverse osmosis concentration adopts is polysulfones, polyethersulfone, complex reverse osmosis membrane, its working conditions be temperature at 30 ~ 35 DEG C, operating pressure 2.0 ~ 4.0Mpa.
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And these belong to spirit institute's apparent change of extending out of the present invention or change and are still among protection scope of the present invention.
Claims (1)
1. a production method for furfural, is characterized in that: through ceramic membrane filter removal of impurities, obtains thick liquid after slagging-off; Enter continuous fluid tripping device afterwards, carry out continuous ionic exchange, from continuous fluid tripping device, solution out concentrates through reverse osmosis system again, obtains concentrated solution; Concentrated solution is sent into hydrolysis system, the furfural gas obtained sends into fore-running and rectification working process, furfural finished product is obtained after rectifying, wherein ceramic membrane equips the aperture of the ceramic membrane adopted is 5-15nm, its working conditions is: between temperature 32-35 DEG C, pressure 0.6-1.0Mpa, and the feature of the reverse osmosis membrane that reverse osmosis concentration adopts is polysulfones, polyethersulfone, complex reverse osmosis membrane, its working conditions be temperature at 30 ~ 35 DEG C, operating pressure 2.0 ~ 4.0Mpa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410617723.6A CN104557813A (en) | 2014-11-05 | 2014-11-05 | Furfural production method |
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| CN201410617723.6A CN104557813A (en) | 2014-11-05 | 2014-11-05 | Furfural production method |
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| CN104557813A true CN104557813A (en) | 2015-04-29 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103709128A (en) * | 2013-11-26 | 2014-04-09 | 河南汇隆化工有限公司 | Furfural purification method |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103709128A (en) * | 2013-11-26 | 2014-04-09 | 河南汇隆化工有限公司 | Furfural purification method |
Non-Patent Citations (1)
| Title |
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| 别士霞等: "《糠醛分离技术研究进展》", 《化工中间体》 * |
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Application publication date: 20150429 |