CN104557810A - Method for producing furfuraldehyde from pentose solution by adopting impinging stream reactor - Google Patents
Method for producing furfuraldehyde from pentose solution by adopting impinging stream reactor Download PDFInfo
- Publication number
- CN104557810A CN104557810A CN201310503565.7A CN201310503565A CN104557810A CN 104557810 A CN104557810 A CN 104557810A CN 201310503565 A CN201310503565 A CN 201310503565A CN 104557810 A CN104557810 A CN 104557810A
- Authority
- CN
- China
- Prior art keywords
- furfural
- acetic acid
- reaction
- furfuraldehyde
- formic acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for producing furfuraldehyde from pentose solution by adopting an impinging stream reactor. The method for producing furfuraldehyde from pentose solution by adopting the impinging stream reactor comprises the following steps: introducing pentose solution and an extraction agent into an impinging stream reactor, reacting under the condition that furfuraldehyde is generated by virtue of pentose, cooling reaction effluent, and layering, wherein an aqueous phase is formed at an upper layer, an extraction phase is formed at a lower layer, the aqueous phase can be recycled as water for hydrolysis of hemicellulose, the extraction phase enters an extraction agent regenerating tower to be further separated, phase splitting is carried out on products at tower top to obtain recycled extraction agent and a small amount of recycled water, the extraction agent can be recycled, products at the bottom of the regenerating tower enter a furfuraldehyde finished product tower to be further separated, acetic acid and formic acid are obtained at the top of the furfuraldehyde finished product tower, and furfuraldehyde is obtained at the bottom of the furfuraldehyde finished product tower; and acetic acid and formic acid enter an acetic acid refining tower to be further separated, formic acid is obtained at the top of the acetic acid refining tower, and acetic acid is obtained at the bottom of the acetic acid refining tower. The method for producing furfuraldehyde from pentose solution by adopting the impinging stream reactor has the advantages that the impinging stream reactor is adopted for producing furfuraldehyde, mass transfer rate is high, side reaction is hardly carried out, and yield of furfuraldehyde is increased; meanwhile, furfuraldehyde, acetic acid and formic acid are recycled, and no waste liquid is discharged, so that the method for producing furfuraldehyde from pentose solution by adopting the impinging stream reactor is an environment-friendly technology.
Description
Technical field
The present invention relates to and a kind ofly produce the method for furfural by pentose solution, particularly a kind ofly adopt high efficient mixed reactor to produce furfural and the method for by-product formic acid and acetic acid simultaneously.
Background technology
Furfural, has another name called furtural.Owing to there is the functional groups such as aldehyde radical, diene, cyclic ethers in Furfural Molecule structure, so it has the character of aldehyde, ether, diene and arene compound concurrently, the reaction of number of different types can be participated in, synthesize multiple Chemicals, be widely used in multiple production fields such as food, medicine, synthetic resins, casting.
The raw material of current production furfural is the vegetable fibre being rich in piperylene, as corn cob, bagasse, cornstalk, rice husk etc.Its principle is that first piperylene is hydrolyzed to pentose, and then dehydration of pentoses cyclisation generates furfural.
According to pentosan hydralysis and this two-step reaction of dehydration of pentoses whether in same reactor, furfural production method can be divided into single stage method and two-step approach.The advantage of single stage method is that equipment is simple, simple to operate, but it is large that its main drawback is steam consumption, produce the steam that 1 ton of furfural consumes 18 ~ 24 tons, furaldehyde yield is low, only have about 45%, produce a large amount of waste water and dregs, produce 1 ton of furfural and produce 24 tons of high pollution waste water, raw material availability is low, produce 1 ton of furfural, consume corn cob 11 tons, waste residue turns black, and Mierocrystalline cellulose and xylogen destroy serious.Two-step approach is produced furfural technology due to pentosan hydralysis and dehydration of pentoses and is carried out in two reactors, the raw material availability that can solve existing furfural production is low, raw material sources are narrow, furaldehyde yield is low, processing wastewater is difficult, furfural dregs is difficult to continue the difficult problems such as utilization, and this method is considered to the furfural production novel method of most prospect.
" two-step approach " produces the first step in furfural technology at present; namely to produce pentose technology ripe in biomass material hydrolysis; under relatively mild reaction conditions; hemicellulose in biomass and hydrolyzable mainly generate pentose; ethanoyl simultaneously on half fiber molecule side chain and the oxidized generation acetic acid of formyl radical and formic acid, therefore in pentose solution also containing a certain amount of formic acid and acetic acid.But produce furfural process by pentose, due to furfural easily and its precursor generation side reaction thus cause furaldehyde yield very low, this also becomes " two-step approach " generates furfural technology and fails the basic reason of industrial application.
Only while pentose reaction generates furfural, fast the furfural fast transfer that reaction generates is gone out reaction system and fundamentally could reduce side reaction raising furaldehyde yield.Reaction, extraction is produced the pentose that furfural technology is considered to most industrial prospect and is produced furfural technology.Reaction, extraction is produced furfural technology and is referred to that generating furfural process in pentose reaction adds a kind of not dissolving each other with water and furfural is had to the solvent of highly selective, constantly furfural is extracted into solvent phase from water react system by solvent, thus greatly reduces side reaction raising furaldehyde yield.
CN101486695A discloses the method and apparatus that a kind of reaction, extraction prepares furfural.This invention take supercritical co as extraction agent, take solid acid as catalyzer, supercritical co and pentose solution counter current contact in packed extraction tower is reacted, temperature of reaction be 200 DEG C, xylose concentration 30% (wt), supercritical co pressure be 7 MPa time, furaldehyde yield is 70%.
CN102627618A discloses a kind of method that reaction, extraction produces furfural.This invention utilizes organic solvent and pentose solution counter current contact in packed extraction tower to react, temperature of reaction be 200 DEG C, pentose sugar concentration 1.56% (wt), solvent ratio 3:1 time, furaldehyde yield is 70%.
Adopt reaction, extraction technique to prepare in the process of furfural, pentose solution and extraction agent can mix efficiently contact to impel react the furfural that generates enough fast mass transfer be restrict furaldehyde yield most critical factor just to extraction phase.In above-mentioned patent, extraction agent and pentose solution are all counter current contact reactions in packed extraction tower, but packing tower mixed effect is poor, and side reaction seriously causes furaldehyde yield lower, and the highest only have 70%; The surface that the condensation product that side reaction generates also can be accumulated in filler causes filler to block, and production process cannot be carried out for a long time; Foregoing invention method cannot reclaim acetic acid and the formic acid of pentose solution simultaneously in addition, if the direct discharge of the aqueous solution reacted not only can cause serious environmental pollution, also can cause the waste of precious resources.
summary of the invention
For the deficiencies in the prior art, the invention provides a kind of use impact flow reactor, High-efficient Production furfural also reclaims the novel method of byproduct formic acid and acetic acid simultaneously.
The invention provides a kind of impact flow reactor that adopts and produce the method for furfural by pentose solution, comprise following content:
(1) take pentose solution as raw material, impact flow reactor is adopted to produce the reactor of furfural as pentose reaction, pentose solution and extraction agent are passed into impact flow reactor respectively by handling equipment, reaction used catalyst is formic acid and/or acetic acid, carries out mixing and contacting reaction under generating the reaction conditions of furfural at dehydration of pentoses;
(2) reaction effluent that step (1) obtains carries out cooling stratification, and upper strata is aqueous phase, the unreacted pentose of the furfural containing trace, acetic acid, formic acid and trace, and lower floor is extraction phase, the moisture mainly containing furfural, acetic acid, formic acid and trace;
(3) extraction phase that step (2) obtains enters extractant regeneration tower and is separated, and overhead product obtains the extraction agent of regeneration and a small amount of water through phase-splitting, and tower reactor obtains the mixture of water-free furfural, acetic acid and formic acid;
(4) in step (3), tower reactor gained furfural, acetic acid enter furfural finishing column with the mixture of formic acid and are separated, and tower reactor obtains furfural, and tower top obtains acetic acid and formic acid mixtures;
(5) acetic acid that in step (4), tower top obtains and formic acid mixtures enter acetic acid refining tower, and tower top obtains formic acid, and tower reactor obtains acetic acid.
It is 150 ~ 280 DEG C that dehydration of pentoses of the present invention generates furfural reaction temperature, is preferably 180 ~ 220 DEG C; Reaction time is 0.1 ~ 2 h.
The present invention, under reaction pressure should be greater than temperature of reaction, aqueous phase bubbling pressure is to ensure that reaction is carried out under liquid phase state, and reaction pressure scope is at 2 ~ 10 MPa, and preferred pressure is 2 ~ 6 MPa.
In the inventive method, extraction agent used is composite extractant, comprises the hydrochloric ether that benzene, vinyl acetic monomer and boiling point are less than formic acid boiling point.Wherein, benzene 10wt% ~ 60wt%, vinyl acetic monomer 10wt% ~ 30wt%, hydrochloric ether 10wt% ~ 60wt%.Be preferably benzene 20 ~ 40wt%, vinyl acetic monomer 15 ~ 25wt%, hydrochloric ether 20 ~ 40wt%.Described hydrochloric ether is the mixture of one or more in trichloromethane, trieline, 1，1，1-trichloroethane, vinyl trichloride.
In the inventive method, composite extractant also plays the effect of entrainer simultaneously, and in extractant regeneration tower, extraction agent and water form azeotrope and the moisture in furfural and mixture of carboxylic acids is taken to tower top.
In the inventive method, can also add a certain amount of inorganic salt in described pentose solution, can be specifically one or more in sodium sulfate, calcium sulfate, sodium-chlor, SODIUMNITRATE, preferably sulfuric acid sodium and/or sodium-chlor.Described inorganic salt consumption is the 1wt% ~ 5wt% of pentose solution.
In the inventive method, dehydration of pentoses catalysts is preferably acetic acid and formic acid, and described catalyst levels is the 1wt% ~ 5wt% of pentose solution.
The impact flow reactor that the present invention relates to can use for liquid reactive various types of impact flow reactor in prior art, can according to the scale of the scale of device and operational condition determination impact flow reactor.For improving the mixed effect of impact flow reactor, can set up Matter Transfer between impact flow reactor outlet and entrance, circulated material quantity is 5% ~ 500% of inlet amount.
The inventive method adopt impact flow reactor be the production unit that reaction, extraction produces furfural technique, material is moved to middle part by guide shell, and clashes in opposite directions at this place, impact surface and around form impingement region.In this district from violent relative movement between the stream group of different directions make between stream group with liquid phase between effective mixing and contact, while pentose reaction generates furfural, strengthening furfural mass transfer process, makes furfural equilibrium establishment instantaneously between aqueous phase and extraction agent.After shock, the ring casing of fluid through between guide shell and container inner wall returns to the two ends, left and right of container respectively, is then fed respectively again and is conducted through guide shell flow direction middle part, two, left and right and again clashes into, iterative cycles like this.Make pentose solution and extraction agent reach the object mixed, thus improve rate of mass transfer, greatly reduce the generation of producing side reaction in furfural process, improve furaldehyde yield, can as a kind of novel method of continuous seepage furfural.
In the inventive method, have employed double solvents as extraction agent, wherein, vinyl acetic monomer all has very high selectivity to formic acid, acetic acid and furfural, benzene and hydrochloric ether all have very high selectivity to furfural, benzene and hydrochloric ether are water-soluble hardly and Dichlorodiphenyl Acetate ethyl ester has very high selectivity, and vinyl acetic monomer can be made water-soluble hardly, solve vinyl acetic monomer because of in water solubleness large and can not as the problem of extraction agent; Hydrochloric ether can also play the effect regulating composite extractant density and viscosity simultaneously; This composite extractant all has very high selectivity to furfural, acetic acid and formic acid, byproduct formic acid and acetic acid can be reclaimed while reaction, extraction produces furfural, furaldehyde yield is greater than 80%, and acetic acid and the formic acid rate of recovery are greater than 90%, and the aqueous phase reacted can be used as system reuse water.
The inventive method, in the composite extractant adopted, benzene and vinyl acetic monomer all can form azeotrope with water, therefore composite extractant can also play the entrainer effect of dehydration, this makes dehydration of the present invention need not add other entrainer, so present invention process flow process is simple, and be separated the furfural that obtains and acetate products purity high.
The inventive method, by adding a certain amount of inorganic salt in aqueous phase, inorganic salt greatly reduce the mutual solubility of extraction agent and aqueous phase under high temperature, solve at high temperature because extraction agent and water mutual solubility cause extraction agent to lose seriously greatly, finally cause reaction, extraction technique industrially cannot apply this key technical problem; Inorganic salt both had stronger catalytic activity to dehydration of pentoses reaction in addition, substantially increased again the selectivity of extraction agent to furfural, formic acid and acetic acid, contributed to reducing side reaction and improved furaldehyde yield.
The present invention generates the reaction mechanism of furfural by the reaction of research pentose, finds that pentose is under reaction generates furfural condition, furfural very easily with its precursor generation side reaction, this is the basic reason causing furaldehyde yield low.Tradition reaction, extraction is produced furfural technology and is often carried out in packing tower, aqueous phase and extraction agent mixed effect very poor, make furfural cannot be delivered to extraction phase enough fast, this causes furaldehyde yield still very low.Therefore, the present invention adopts impact flow reactor to produce the reactor of furfural technique as reaction, extraction, enhances microcosmic mixing and microcosmic mass transfer greatly, makes furfural reach partition equilibrium instantaneously at extraction agent and water two-phase, reduce side reaction, improve furaldehyde yield.Solve because of extraction agent and pentose solution mixed effect poor, reaction system is two-phase, and the side reaction that furfural causes far above furfural content during biphase equilibrium at water react system concentration is serious, furaldehyde yield is low and the problem such as reactor plugs.Simplify technical process, reduce production cost and facility investment.Without discharging of waste liquid in production process, it is an environmental protection processing method.
Accompanying drawing explanation
Fig. 1 is impact flow reactor structural representation of the present invention.
Fig. 2 is a kind of process flow diagram of the inventive method.
Embodiment
As shown in Figure 1, impact flow reactor of the present invention comprises: be arranged on nearly two ends place in the middle part of container 4 respectively symmetrically and be submerged in material two guide shells 3,5 and respectively coaxially and two feed-pipes 1,7 be arranged on symmetrically in two guide shells.Loading process stream in container 4, is the useful volume district of reaction, and in order to improve flow efficiency, the circular cylindrical shell of container 4 makes.Under the promotion of the material of the material in guide shell in two feed-pipes respectively from two ends through guide shell 3,5 high speed flow to container 4 center, and to clash in opposite directions in center, around impact surface, form impingement region.Make effectively contact and mix between stream group with between liquid phase from violent relative movement between the stream group of different directions in this district.After shock, the ring casing of fluid through between guide shell 3,5 and container 4 inwall returns to two ends, and the mass transport be then fed again in pipe 1,7 flows to container 4 center by guide shell 3,5 and again clashes into, iterative cycles like this, discharges by exporting 2,6.This perfect mixing effect of circulation in opposite directions, makes pentose solution and extraction agent reach the object mixed, thus improves rate of mass transfer, reduces side reaction, improves furaldehyde yield.The recycle stock handling equipment (as pump) of impact flow reactor can adopt one or several.
As shown in Figure 2, materials abstraction agent 8 and the pentose solution 9 of reaction will be participated according to stoichiometric ratio, with pump or other equipment for liquid transportation, material is input in tundish 10 respectively, carry out pre-mixing, then by pump or other equipment for liquid transportation, be input to the opening for feed 12 of impact flow reactor 4, 13, feed stream flows to container center through guide shell at a high speed under pressure, and clash in opposite directions in center, impingement region is formed around impact surface, material after clashing into is from two side outlets 14, 15 flow to tundish 10, the opening for feed 12 of impact flow reactor is input to again by pump, 13, again clash into, reactor pressure is controlled by pressure-regulator 16.Directly enter phase separation tank 17 from the reaction mass of pressure-regulator 16 discharge and carry out cooling stratification, upper strata is the aqueous phase 18 reacted, aqueous phase 18 can be used as hydrolysis of hemicellulose water, lower floor is for being rich in furfural, the extraction phase 19 of acetic acid and formic acid, lower floor's extraction phase 19 directly enters extractant regeneration tower 20 and is separated, overhead product 21 is the extraction agent of regeneration and a small amount of water, extraction agent can be recycled, bottom product 22 is water-free furfural and mixture of carboxylic acids, then bottom product 22 directly enters furfural finishing column 23 and is separated, furfural product 24 is obtained at the bottom of tower, purity is greater than 99.5%, overhead product 25 is formic acid and vinegar stock, overhead product 25 enters acetic acid refining tower 26 and is separated, tower top obtains formic acid product 27, its purity is greater than 99.5%, acetate products 28 is obtained at the bottom of tower, its purity is greater than 99.5%.
Method of the present invention and effect is further illustrated below by embodiment.The percentage composition related to is mass percentage.
In embodiment, pentose transformation efficiency, furaldehyde yield and acid recovering rate are calculated by following formula.
Embodiment 1
In raw material pentose solution, furfural, acetic acid, formic acid concn are respectively 4.9wt%, 3.1wt%, 0.6wt%, sodium sulfate concentration 3wt%.
Extraction agent is benzene, vinyl acetic monomer, 1，1，1-trichloroethane mixed solvent, and wherein, benzene accounts for 40wt%, and vinyl acetic monomer accounts for 20wt%, and 1，1，1-trichloroethane accounts for 40wt%.
Extraction agent and pentose solution charge ratio are 3:1 (volume ratio), and the feeding rate of extraction agent and pentose solution equals impact flow reactor volume, and (namely feed volume air speed is 1h
-1namely, also the reaction times is 1 h), squeezes in impact flow reactor respectively by extraction agent and pentose solution with pump, and to react-extraction process with recycle stock short mix in impact flow reactor, recycle stock speed is 200% of inlet amount.Controlling temperature of reaction is 200 DEG C, and reaction pressure is 3 MPa.
Experimental result shows that pentose transformation efficiency is 97.4%, and furaldehyde yield is 82.1%, and recovery rate is 90.9%, and the formic acid rate of recovery is 89.8%.
Embodiment 2
According to the method for embodiment 1,2 times of difference to be feeding rate be impact flow reactor volume, namely the reaction times is 0.5 h.
Experimental result shows that pentose transformation efficiency is 78.1%, and furaldehyde yield is 61.4%, and recovery rate is 93.8%, and the formic acid rate of recovery is 90.8%.
Embodiment 3
According to the method for embodiment 1,0.67 times of difference to be feeding rate be impact flow reactor volume, namely the reaction times is 1.5 h.
Experimental result shows that pentose transformation efficiency is 99%, and furaldehyde yield is 82.5%, and recovery rate is 93.9%, and the formic acid rate of recovery is 90.9%.
Embodiment 4
According to the method for embodiment 1, difference is recycle stream is 100% of inlet amount.
Experimental result shows that pentose transformation efficiency is 96.8%, and furaldehyde yield is 82.1%, and recovery rate is 92.3%, and the formic acid rate of recovery is 90.7%.
Embodiment 5
According to the method for embodiment 1, difference is recycle stream is 300% of inlet amount.
Experimental result shows that pentose transformation efficiency is 96.1%, and furaldehyde yield is 81.1%, and recovery rate is 93.4%, and the formic acid rate of recovery is 91.3%.
Embodiment 6
According to the method for embodiment 1, difference is that temperature of reaction becomes 180 DEG C.
Experimental result shows that pentose transformation efficiency is 45.5%, and furaldehyde yield is 38.7%, and recovery rate is 94.6%, and the formic acid rate of recovery is 92.7%.
Embodiment 7
According to the method for embodiment 1, difference is that temperature of reaction becomes 220 DEG C.
Experimental result shows that pentose transformation efficiency is 99.5%, and furaldehyde yield is 84.1%, and recovery rate is 93.7%, and the formic acid rate of recovery is 91.4%.
Embodiment 8
According to the method for embodiment 1, difference is sodium sulfate concentration vanishing.
Experimental result shows that pentose transformation efficiency is 94.1%, and furaldehyde yield is 76.4%, and recovery rate is 82.5%, and the formic acid rate of recovery is 81.4%.
Embodiment 9
According to the method for embodiment 1, difference is that sodium sulfate concentration becomes 5%.
Experimental result shows that pentose transformation efficiency is 97.8%, and furaldehyde yield is 83.5%, and recovery rate is 93.9%, and the formic acid rate of recovery is 93.1%.
Embodiment 10
According to the method for embodiment 1, difference is that extraction agent and pentose solution charge ratio become 1:1.
Experimental result shows that pentose transformation efficiency is 97.9%, and furaldehyde yield is 77.3%, and recovery rate is 83.5%, and the formic acid rate of recovery is 79.7%.
Embodiment 11
According to the method for embodiment 1, difference is that extraction agent and pentose solution charge ratio become 5:1.
Experimental result shows that pentose transformation efficiency is 97.5%, and furaldehyde yield is 85.3%, and recovery rate is 94.5%, and the formic acid rate of recovery is 92.8%.
Embodiment 12:
According to the method for embodiment 1, difference is that composite extractant composition becomes: benzene, vinyl acetic monomer, 1，1，1-trichloroethane mass ratio 3:1:1.
Experimental result shows that pentose transformation efficiency is 97.7%, and furaldehyde yield is 77.3%, and recovery rate is 85.5%, and the formic acid rate of recovery is 82.5%.
Embodiment 13:
According to the method for embodiment 1, difference is that composite extractant composition becomes: benzene, vinyl acetic monomer, 1，1，1-trichloroethane mass ratio 1:1:3.
Experimental result shows that pentose transformation efficiency is 97.8%, and furaldehyde yield is 82.7%, and recovery rate is 81.5%, and the formic acid rate of recovery is 79.8%.
Embodiment 14:
According to the method for embodiment 1, difference is that composite extractant composition becomes: benzene, vinyl acetic monomer, 1，1，1-trichloroethane mass ratio 1:0:1.
Experimental result shows that pentose transformation efficiency is 97.8%, and furaldehyde yield is 83.4%, and recovery rate is 71.9%, and the formic acid rate of recovery is 70.8%.
Embodiment 15:
According to the method for embodiment 1, difference is that composite extractant composition becomes: benzene, vinyl acetic monomer, 1，1，1-trichloroethane mass ratio 0:1:1.
Experimental result shows that pentose transformation efficiency is 97.7%, and furaldehyde yield is 73.8%, and recovery rate is 92.9%, and the formic acid rate of recovery is 89.8%.
[0055] embodiment 16:
According to the method for embodiment 1, difference is that composite extractant composition becomes: benzene, vinyl acetic monomer, 1，1，1-trichloroethane mass ratio 1:1:0.
Experimental result shows that pentose transformation efficiency is 97.8%, and furaldehyde yield is 76.1%, and recovery rate is 89.5%, and the formic acid rate of recovery is 85.9%.
Claims (13)
1. adopt impact flow reactor to produce a method for furfural by pentose solution, comprise following content:
(1) take pentose solution as raw material, impact flow reactor is adopted to produce the reactor of furfural as pentose reaction, pentose solution and extraction agent are passed into impact flow reactor respectively by handling equipment, reaction used catalyst is formic acid and/or acetic acid, carries out mixing and contacting reaction under generating the reaction conditions of furfural at dehydration of pentoses;
(2) reaction effluent that step (1) obtains carries out cooling stratification, and upper strata is aqueous phase, the unreacted pentose of the furfural containing trace, acetic acid, formic acid and trace, and lower floor is extraction phase, the moisture mainly containing furfural, acetic acid, formic acid and trace;
(3) extraction phase that step (2) obtains enters extractant regeneration tower and is separated, and overhead product obtains the extraction agent of regeneration and a small amount of water through phase-splitting, and tower reactor obtains the mixture of water-free furfural, acetic acid and formic acid;
(4) in step (3), tower reactor gained furfural, acetic acid enter furfural finishing column with the mixture of formic acid and are separated, and tower reactor obtains furfural, and tower top obtains acetic acid and formic acid mixtures;
(5) acetic acid that in step (4), tower top obtains and formic acid mixtures enter acetic acid refining tower, and tower top obtains formic acid, and tower reactor obtains acetic acid.
2. in accordance with the method for claim 1, it is characterized in that: it is 150 ~ 280 DEG C that dehydration of pentoses generates furfural reaction temperature, and reaction time is 0.1 ~ 2 h.
3. in accordance with the method for claim 2, it is characterized in that: it is 180 ~ 220 DEG C that dehydration of pentoses generates furfural reaction temperature.
4. in accordance with the method for claim 1, it is characterized in that: under reaction pressure is greater than temperature of reaction, aqueous phase bubbling pressure is to ensure that reaction is carried out under liquid phase state, and reaction pressure is 2 ~ 10MPa.
5. in accordance with the method for claim 4, it is characterized in that: reaction pressure is 2 ~ 6MPa.
6. in accordance with the method for claim 1, it is characterized in that: described catalyst levels is the 1wt% ~ 5wt% of pentose solution.
7. in accordance with the method for claim 1, it is characterized in that: extraction agent is composite extractant, comprise the hydrochloric ether that benzene, vinyl acetic monomer and boiling point are less than formic acid boiling point.
8. in accordance with the method for claim 7, it is characterized in that: described hydrochloric ether is one or more in trichloromethane, trieline, 1，1，1-trichloroethane, vinyl trichloride.
9. in accordance with the method for claim 1, it is characterized in that: in composite extractant, benzene is 10wt% ~ 60wt%, vinyl acetic monomer is 10wt% ~ 30wt%, and hydrochloric ether is 10wt% ~ 60wt%.
10. in accordance with the method for claim 9, it is characterized in that: in composite extractant, benzene is 20wt% ~ 40wt%, vinyl acetic monomer is 15wt% ~ 25wt%, and hydrochloric ether is 20wt% ~ 40wt%.
11. in accordance with the method for claim 1, it is characterized in that: add inorganic salt in described pentose solution, and described inorganic salt consumption is the 1wt% ~ 5wt% of pentose solution.
12. in accordance with the method for claim 11, it is characterized in that: inorganic salt are one or more in sodium sulfate, calcium sulfate, sodium-chlor, SODIUMNITRATE.
13. in accordance with the method for claim 12, it is characterized in that: inorganic salt are sodium sulfate and/or sodium-chlor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310503565.7A CN104557810A (en) | 2013-10-24 | 2013-10-24 | Method for producing furfuraldehyde from pentose solution by adopting impinging stream reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310503565.7A CN104557810A (en) | 2013-10-24 | 2013-10-24 | Method for producing furfuraldehyde from pentose solution by adopting impinging stream reactor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104557810A true CN104557810A (en) | 2015-04-29 |
Family
ID=53074983
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310503565.7A Pending CN104557810A (en) | 2013-10-24 | 2013-10-24 | Method for producing furfuraldehyde from pentose solution by adopting impinging stream reactor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104557810A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948010A (en) * | 2016-04-27 | 2016-09-21 | 四川大学 | Impinging stream reinforced wet-process phosphoric acid extraction method and device |
| CN110563675A (en) * | 2019-08-01 | 2019-12-13 | 四川金象赛瑞化工股份有限公司 | Method for preparing furfural by extracting xylose through steam explosion of cotton stalks and full utilization |
| JP2021535901A (en) * | 2019-03-27 | 2021-12-23 | 広州楹鼎生物科技有限公司 | How to prepare furfural |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627618A (en) * | 2012-03-22 | 2012-08-08 | 天津大学 | Method for producing furfural through biomass hydrolysis-reactive extraction |
-
2013
- 2013-10-24 CN CN201310503565.7A patent/CN104557810A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627618A (en) * | 2012-03-22 | 2012-08-08 | 天津大学 | Method for producing furfural through biomass hydrolysis-reactive extraction |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948010A (en) * | 2016-04-27 | 2016-09-21 | 四川大学 | Impinging stream reinforced wet-process phosphoric acid extraction method and device |
| JP2021535901A (en) * | 2019-03-27 | 2021-12-23 | 広州楹鼎生物科技有限公司 | How to prepare furfural |
| JP7100925B2 (en) | 2019-03-27 | 2022-07-14 | 広州楹鼎生物科技有限公司 | How to prepare furfural |
| CN110563675A (en) * | 2019-08-01 | 2019-12-13 | 四川金象赛瑞化工股份有限公司 | Method for preparing furfural by extracting xylose through steam explosion of cotton stalks and full utilization |
| CN110563675B (en) * | 2019-08-01 | 2023-05-30 | 四川金象赛瑞化工股份有限公司 | Method for preparing furfural and fully utilizing xylose by cotton stalk steam explosion extraction |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107118083B (en) | Device and method for refining and separating polymethoxy dimethyl ether containing formaldehyde | |
| CN104557809A (en) | Method for producing furfural from pentose | |
| CN103333047B (en) | Preparation method of dichloropropanol | |
| CN103992206B (en) | The method and system of prenol are prepared in a kind of ester exchange | |
| CN111848557A (en) | Preparation process of furfural | |
| CN109081767A (en) | A kind of the synthesis rectification technique and its equipment of monochloro methane | |
| CN107033107A (en) | A kind of method for preparing epoxychloropropane | |
| CN107311868B (en) | Method for preparing p-tert-butyl methyl benzoate | |
| CN114315767A (en) | Preparation method and preparation device of 5-hydroxymethylfurfural | |
| CN104557810A (en) | Method for producing furfuraldehyde from pentose solution by adopting impinging stream reactor | |
| CN104557812A (en) | Method for producing furfural from biomass | |
| CN104557807A (en) | Production process of 5-hydroxymethyl furfural | |
| CN103172600A (en) | Preparation method of furfuraldehyde | |
| CN106146434A (en) | A kind of preparation technology of 5 hydroxymethyl furfural | |
| CN106146441A (en) | A kind of preparation technology of furfural | |
| CN106146439A (en) | A kind of preparation method of furfural | |
| CN104557805A (en) | Method for producing 5-hydroxymethyl furfural | |
| CN101318945B (en) | Method for preparing furfurol with poly-pentose containing waste agronomic crop as raw material | |
| CN110407780A (en) | A kind of refining methd of furfural | |
| CN109439706A (en) | A method of producing 5 hydroxymethyl furfural | |
| CN110498782B (en) | Continuous preparation method of 2, 5-dimethyl-4-hydroxy-3 (2H) furanone | |
| CN105480948A (en) | Method and system for recycling by-product hydrogen chloride in fatty acid or fatty acyl chloride chlorination production process | |
| CN212076906U (en) | Side-line reaction type dioxolane production process device | |
| CN104557806A (en) | Preparation method of 5-hydroxymethylfurfural | |
| CN104557811A (en) | Method for producing furfural from pentose solution by adopting ultrasonic reactor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150429 |