CN208055237U - The system for continuously preparing furfural with the pentose solution containing acid - Google Patents
The system for continuously preparing furfural with the pentose solution containing acid Download PDFInfo
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- CN208055237U CN208055237U CN201721684194.7U CN201721684194U CN208055237U CN 208055237 U CN208055237 U CN 208055237U CN 201721684194 U CN201721684194 U CN 201721684194U CN 208055237 U CN208055237 U CN 208055237U
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- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 title claims abstract description 299
- 239000002253 acid Substances 0.000 title claims abstract description 90
- 150000002972 pentoses Chemical class 0.000 title claims abstract description 52
- 239000007788 liquid Substances 0.000 claims abstract description 81
- 238000006243 chemical reaction Methods 0.000 claims abstract description 65
- 238000000746 purification Methods 0.000 claims abstract description 25
- 238000004821 distillation Methods 0.000 claims description 83
- 239000002994 raw material Substances 0.000 claims description 25
- 150000001299 aldehydes Chemical class 0.000 claims description 21
- 238000000926 separation method Methods 0.000 claims description 20
- 239000008346 aqueous phase Substances 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- 239000012071 phase Substances 0.000 claims description 15
- 238000010992 reflux Methods 0.000 claims description 12
- 239000002351 wastewater Substances 0.000 claims description 11
- 150000003839 salts Chemical class 0.000 claims description 9
- 238000004064 recycling Methods 0.000 claims description 8
- 238000006210 cyclodehydration reaction Methods 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 5
- 230000003472 neutralizing effect Effects 0.000 claims description 3
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 6
- 230000002378 acidificating effect Effects 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000013461 design Methods 0.000 abstract description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 2
- 239000011707 mineral Substances 0.000 abstract description 2
- 238000007086 side reaction Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 23
- 238000000605 extraction Methods 0.000 description 13
- 239000000047 product Substances 0.000 description 13
- 239000003921 oil Substances 0.000 description 10
- 235000019198 oils Nutrition 0.000 description 10
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 229920002488 Hemicellulose Polymers 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 230000018044 dehydration Effects 0.000 description 4
- 238000006068 polycondensation reaction Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 3
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000004939 coking Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000007171 acid catalysis Methods 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 235000014633 carbohydrates Nutrition 0.000 description 2
- 239000007806 chemical reaction intermediate Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- 238000011044 inertial separation Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000066 reactive distillation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The utility model is related to a kind of system continuously preparing furfural with the pentose solution containing acid, which includes stripping reaction tower, separative element and purification unit.It is catalyst that liquid mineral acid, which can be used, in the system of the utility model, and catalytic capability is strong, and reaction temperature is low, additionally it is possible to handle low concentration liquid glucose.The utility model directly strips heating using steam, takes the furfural of generation out of in time with steam while so that pentose is reacted, avoids furfural that side reaction occurs under liquid acidic environment.The utility model reaction process is not necessarily to any extractant, easily separated after the furfural cooling taken away with steam.Whole system reasonable design, furaldehyde yield is high, and specific energy consumption is low.
Description
Technical field
The utility model belongs to furfural production technical field, especially relate to two-step method prepare in furfural with containing acid
Pentose solution continuously prepares the technology of furfural.
Background technology
Furfural (also known as furtural) is a kind of important chemical products, is widely used in synthetic plastic, medicine, pesticide etc.
The demand of industrial circle, annual whole world furfural is very big.Furfural can selectively extract from oil, vegetable oil therein
Unsaturated component can also extract aromatised fraction therein from lubricating oil and diesel oil.With the aggravation and environmental protection of energy crisis
It is required that producing the furfural of high added value using reproducible agriculture and forestry organic waste material, more and more paid attention to by people.
At present at industrial scale, the method that can uniquely obtain furfural is still to pass through hydrolysis using corncob as raw material
Method obtains.According to pentosan hydralysis in corncob hemicellulose and pentose monomers cyclodehydration whether in the same reactor
It carries out, furfural production technology can be divided into one-step method and two-step method again.
One-step method is that the raw material containing hemicellulose is fitted into hydrolyzer, under acid catalysis and certain temperature, makes hemicellulose
Element is hydrolyzed into pentose, while pentose is dehydrated to form furfural again.One-step method is easy to operate because its equipment investment is few, in furfural work
Industry is widely used.But one-step method is uneven since raw material heats, and furaldehyde yield is low, large steam consumption, and environmental pollution is serious.
Two-step method is that the dehydration of the hydrolysis of hemicellulose and pentose is divided into two steps, respectively in different equipment
Middle completion, reaction equation are as follows：
Currently, first step hydrolysis of hemicellulose produce pentose high income, but in second step dehydration of pentoses cyclization process due to
The decomposition reaction of furfural itself and polycondensation reaction with reaction intermediate so that furaldehyde yield is relatively low, therefore dehydration of pentoses ring
The decomposition reaction and polycondensation reaction that furfural how is reduced in step changed, the yield for improving furfural is the key that two-step method.Due to Europe
Mei Deng developed countries stop furfural production already, therefore report the research of furfural technology seldom.
103339119 A of patent CN disclose one kind without using heterogeneous catalyst, by using continuous pipe
Formula reactor is to dissolving xylose progress liquid-phase dehydration reaction in a solvent.But in the method, the furfural of generation cannot in time from
Open reaction system so that cross polymerization reaction occurs between furfural and raw material xylose and reaction intermediate, and furfural can also
Further degradation generates ketone, aldehyde etc., reduces the selectivity that xylose generates furfural.
102690248 A of patent CN disclose a kind of pentose solution in the system for having extractant, and continuous countercurrent extraction generates
Furfural.Although the method can make furfural be detached from acid reaction environment in time, the selectivity of furfural, extractant valence used are improved
Lattice are expensive, and toxicity is big, and wastewater treatment is complicated, and the recycling of extractant needs to consume big energy, complex operation,
Equipment investment is high.
Patent CN102584751 B describe a kind of technique that reaction rectification method prepares furfural.Using organic in the patent
Sour formic acid and acetic acid are as catalyst.Since organic acid catalysis effect is poor, higher reaction temperature and reaction pressure are needed.Most
Crucially the mode of reactive distillation tower reactor indirectly heat provides heat, due to usually containing salt and its in the solution containing pentose
His carbohydrate impurity, under acidic environment and when heat exchanger heat exchange, heat exchanger surface is easy coking so that react cannot continuously into
Row.
Utility model content
The utility model is proposed in view of above-mentioned the problems of the prior art.The utility model provides a kind of with containing
The pentose solution system that continuously prepares furfural of acid, solves at least that furaldehyde yield in the prior art is low, and byproduct of reaction is more,
The problems such as production cost is high, low production efficiency, environmental pollution is serious, can effectively improve furaldehyde yield, avoid pair as far as possible
Reaction occurs, and specific energy consumption is low, and environmental pollution is small.
One side according to the present utility model provides a kind of system continuously preparing furfural with the pentose solution containing acid,
The system includes stripping reaction tower comprising is located at steam (vapor) outlet and first feed(raw material)inlet at top, and the vapour positioned at bottom
Carry steam inlet and acid solution outlet；Wherein, first feed(raw material)inlet is used to receive the pentose solution work containing acid of the first temperature
It is raw material to carry out cyclodehydration reaction, the stripped vapor entrance is used to receive the stripped vapor of second temperature, the steam
Outlet is for providing by the steam containing furfural obtained by the reaction, and the acid solution outlet from bottom of tower for producing acid solution；Separative element,
It is connected with the steam (vapor) outlet, for neutralizing the acid in steam containing furfural, and the salt of gained is detached with steam containing furfural, with
The steam containing furfural that acid content reduces is provided；And purification unit, it is used to purify the furfural of gained.
It is catalyst that liquid mineral acid, which can be used, in the utility model, and catalytic capability is strong, and reaction temperature is low.With solvent extraction
It compares, the utility model can also handle low concentration liquid glucose.The technological process that the utility model is reacted using steam counter-flow stripping,
Reaction process is added without any extractant, and the pentose solution containing acid is contacted with steam from top to bottom, and cyclodehydration reaction is occurring
While generating furfural, the furfural of generation is taken out of by steam, and this avoid furfurals to be sent out for a long time in liquid acidic environment
Raw side reaction.The utility model stripping reaction tower bottom of tower can not set reboiler, and stripping reaction column overhead, which can not be set, to be condensed back to
Flow device；Due to usually containing salt and other carbohydrate impurity in the solution containing pentose, exchange heat in reboiler under acidic environment
It is easy to prevent the coking of reboiler surface and prevent reaction from being carried out continuously, heating is directly stripped using steam and avoids this problem simultaneously
Save equipment investment.Meanwhile the heating of direct steam stripping can also control the residence time of liquid by adjusting quantity of steam, avoid
Overreact.The utility model simplifies furfural production process, and subsequent furfural separation and simple purification are easy, entire technique
Reasonable design, compared with traditional one-step technology, the high 10-30% of furaldehyde yield, the low 10-20% of specific energy consumption.
In a preferred embodiment, separative element can also include filter device, which is used for containing
The steam containing furfural that acid amount reduces is filtered, to provide filtered steam containing furfural.Using for filter device can be further
It removes the impurity in steam containing furfural and effectively reduces the yield of the aldehyde mud in follow-up Furfural Treating Process, extend primary distillation tower again
Boil the service life of device and heat exchange unit.
In a preferred embodiment, which can also include heat exchange unit, the heat exchange unit
Including：Material channel, including the second feed(raw material)inlet, the second feed(raw material)inlet are used to receive penta containing acid of the temperature less than the first temperature
Sugar juice and material outlet, material outlet are connected with the first feed(raw material)inlet, for providing the first temperature to stripping reaction tower
Pentose solution containing acid；And furfural channel, it is mutually isolated with material channel but heat exchange can be carried out, and include that furfural enters
Mouthful, furfural entrance is connected with separative element, is used to receive steam containing furfural and furfural outlet, furfural from separative element and goes out
Mouth is connected with purification unit, for providing furfuryl aldehyde solution.The heat of the steam containing furfural can be effectively utilized using heat exchange unit
Come improve containing acid pentose solution temperature, can faster reach reaction temperature, avoid the waste of energy.
In a preferred embodiment, purification unit may include：Primary distillation tower has the primary distillation tower positioned at middle part
Feed inlet, the primary distillation tower steam (vapor) outlet positioned at top and aqueous phase liquid entrance boil steam inlet and primary distillation tower again positioned at bottom
Bottom liquid exports；Furfuryl aldehyde solution heat exchanger, furfuryl aldehyde solution through furfuryl aldehyde solution heat exchanger be cooled to third temperature through primary distillation tower into
Material mouth enters primary distillation tower；It is furnished with condensation reflux unit equipped with fore-running tower reboiler, tower top in primary distillation tower bottom of tower；Condensation reflux unit packet
Include primary distillation tower condenser and primary distillation tower liquid separation tank；Fore-running tower reboiler becomes after being used to exchange heat a part of bottom liquid boils steaming again
Vapour returns to primary distillation tower through boiling steam inlet again；Primary distillation tower condenser is connected with primary distillation tower steam (vapor) outlet, and being used for will after purification
Steam containing furfural condense to the condensate liquid of the 4th temperature；Primary distillation tower liquid separation tank, is connected with primary distillation tower condenser, for receiving
Condensate liquid carries out liquid separation to obtain aqueous phase liquid and oil phase liquid, and sends aqueous phase liquid back to primary distillation tower through aqueous phase liquid entrance,
It regard oil phase liquid output as chaff aldehyde product.
In a preferred embodiment, separative element may include lye input port to input lye, for neutralizing
Acid in steam containing furfural avoids acid from making furfural decomposition or polycondensation in subsequent processing.
In a preferred embodiment, separative element may include cyclone separator, for steaming salt with containing furfural
Vapour detaches, to provide the steam containing furfural of acid content reduction.Cyclone separator has simple in structure, easy to operate, high temperature resistant, longevity
Order the advantages that long.
In a preferred embodiment, this prepare furfural system can also include acid solution heat exchanger, for receive from
The acid solution of acid solution outlet outflow simultaneously carries out thermal energy recycling.
In a preferred embodiment, purification unit can also include refining plant, for chaff aldehyde product into
Row is dehydrated and takes off light refined to obtain product furfural.
In a preferred embodiment, it can also include waste water evaporator, waste water evaporator that this, which prepares furfural system,
It is connected with the outlet of primary distillation tower bottom liquid, for being steamed to another part bottom liquid exported from primary distillation tower bottom liquid
Hair recycles.
In a preferred embodiment, the first temperature can be set to 80-155 DEG C, and second temperature can be set
It is set to 150-220 DEG C, stripping reaction column overhead temperatures can be set to 140-210 DEG C, and column bottom temperature can be set to
150-220℃.Stripping reaction tower tower top pressure can be set to 0.26-2.2MPa, and tower bottom pressure can be set to 0.37-
2.2MPa.Stripping the temperature and pressure of reaction tower can be adjusted and be arranged by adjusting temperature and pressure of charging etc..
In a preferred embodiment, third temperature can be set to 20-100 DEG C, and the 4th temperature can be set
It is set to 30-90 DEG C, fore-running column overhead temperatures can be set to 100-115 DEG C, and primary distillation tower column bottom temperature can be set to
120-160℃.Primary distillation tower tower top pressure can be set to 0-0.03MPa, and tower bottom pressure can be arranged to 0-
0.35MPa.The temperature and pressure of primary distillation tower can by adjusting charging temperature and pressure, boil ratio, reflux ratio again etc. and adjusted
Section and setting.
In a preferred embodiment, stripping reaction tower bottom of tower can be without reboiler, and stripping reaction column overhead can be with
Frozen-free reflux.
Description of the drawings
The following drawings of the utility model is used to understand the utility model in this as the part of the utility model.Attached drawing
In show the embodiments of the present invention and its description, for explaining the principles of the present invention.
Fig. 1 be described in an embodiment according to the present utility model it is a kind of with containing acid pentose solution continuously prepare chaff
The schematic diagram of the system of aldehyde.
Fig. 2 be described in another embodiment according to the present utility model it is a kind of with containing acid pentose solution continuously prepare
The schematic diagram of the system of furfural.
Specific implementation mode
In the following description, a large amount of concrete details are given more thoroughly to manage in order to provide to the utility model
Solution.It will be apparent, however, to one skilled in the art that the utility model may not need it is one or more of these thin
It saves and is carried out.In other examples, in order to avoid obscuring with the utility model, for more well known in the art
Technical characteristic is not described.
Fig. 1 diagrammatically illustrates an embodiment according to the present utility model.
As shown in Figure 1, it is a kind of system continuously preparing furfural with the pentose solution containing acid, including stripping reaction tower
10, steam (vapor) outlet 11, the first feed(raw material)inlet 12, stripped vapor entrance 13, acid solution outlet 14, separative element 20, purification unit 30.
The device can continuously prepare furfural with following techniques with the pentose solution containing acid.
The pentose solution containing acid being heated by the heaters to the first temperature enters from first raw material at 10 top of stripping reaction tower
Mouth 12 enters in tower, and the stripped vapor of second temperature enters from the stripped vapor entrance 13 of 10 bottom of stripping reaction tower in tower, contains
Cyclodehydration reaction occurs in stripping reaction tower 10 and generates furfural for the pentose solution of acid, and acid is catalyst, then, the chaff of generation
Aldehyde is produced with steam from the steam (vapor) outlet 11 at 10 top of stripping reaction tower, acid solution outlet 14 of the acid solution from 10 bottom of stripping reaction tower
Extraction；The steam containing furfural of extraction enters the separative element 20 being connected with stripping reaction tower 10, and furfural is contained in separative element 20
Acid in steam is neutralized, and obtains the steam containing furfural of acid content reduction；The steam containing furfural that acid content reduces enters and detaches
The connected purification unit 30 of unit 20, and be purified in purification unit 30.
In a preferred embodiment, separative element 20 can also include filter device, and preferably ceramic filter should
Filter device is for being filtered the steam containing furfural that acid content reduces, further to remove the impurity in steam containing furfural.
The use of filter device can effectively reduce the yield of the aldehyde mud in follow-up Furfural Treating Process, extend fore-running tower reboiler and change
The service life of hot cell.
In a preferred embodiment, which can also include heat exchange unit, the heat exchange unit
Including：Material channel and furfural channel.Material channel receives the pentose solution containing acid as raw material, and furfural channel reception, which comes from, to be divided
Steam containing furfural from unit 20.Pentose solution containing acid and steam containing furfural lead to respectively by material channel and furfural channel
It is mutually isolated but can make the pentose solution containing acid and steam containing furfural to carry out heat exchange between road, respectively by gained after heat exchange
Pentose solution containing acid and furfuryl aldehyde solution be sent into stripping reaction tower 10 and purification unit 30.It can be effectively using heat exchange unit
The temperature that the pentose solution containing acid is improved using the heat of the steam containing furfural, can faster be reached reaction temperature, avoided
The waste of energy.
In a preferred embodiment, purification unit 30 may include：Primary distillation tower has the fore-running positioned at middle part
Tower feed inlet, the primary distillation tower steam (vapor) outlet positioned at top and aqueous phase liquid entrance boil steam inlet and fore-running again positioned at bottom
Tower bottom liquid exports；Furfuryl aldehyde solution heat exchanger, furfuryl aldehyde solution are cooled to third temperature through primary distillation tower through furfuryl aldehyde solution heat exchanger
Feed inlet enters primary distillation tower；It is furnished with condensation reflux unit equipped with fore-running tower reboiler, tower top in the primary distillation tower bottom of tower；The condensation
Reflux includes primary distillation tower condenser and primary distillation tower liquid separation tank；A part of bottom liquid becomes after the heat exchange of fore-running tower reboiler
Steam is boiled again returns to primary distillation tower through boiling steam inlet again；Primary distillation tower condenser is connected with primary distillation tower steam (vapor) outlet, and being used for will be pure
Steam containing furfural after change is condensed to the condensate liquid of the 4th temperature；Primary distillation tower liquid separation tank, is connected with primary distillation tower condenser, is used for
The condensate liquid is received, carries out liquid separation to obtain aqueous phase liquid and oil phase liquid, and by the aqueous phase liquid through the water phase liquid
Body entrance sends primary distillation tower back to, regard oil phase liquid output as chaff aldehyde product.
In a preferred embodiment, separative element 20 may include lye input port to input the alkali for neutralization
Liquid avoids acid from making furfural decomposition or polycondensation in subsequent processing to neutralize the acid in steam containing furfural.
In a preferred embodiment, the separation method of separative element 20 can be inertial separation, be separated by filtration, from
One or more of heart separation, the utility model preferably using the cyclone separator of centrifugal separation method is belonged to, be used for by
Salt and solid impurity are detached with steam containing furfural, to provide the steam containing furfural of acid content reduction.Cyclone separator has structure
Be simple and convenient to operate, high temperature resistant, long lifespan the advantages that.
In a preferred embodiment, this prepare furfural system can also include acid solution heat exchanger, for receive from
The acid solution of 14 extraction of acid solution outlet of 10 bottom of stripping reaction tower simultaneously carries out thermal energy recycling.
In a preferred embodiment, purification unit 30 can also include refining plant, for chaff aldehyde product
Be dehydrated and take off light refined to obtain product furfural.
In a preferred embodiment, purification unit 30 further includes waste water evaporator, for discharge primary distillation tower
A part for bottom liquid is evaporated recycling.
In a preferred embodiment, first temperature can be set to 80-155 DEG C, the second temperature
150-220 DEG C is can be set to, stripping 10 tower top temperature of reaction tower can be set to 140-210 DEG C, strip reaction tower 10
Column bottom temperature can be set to 150-220 DEG C, and stripping 10 tower top pressure of reaction tower can be set to 0.26-2.2MPa (tables
Pressure), tower bottom pressure can be set to 0.37-2.2MPa (gauge pressure).The temperature and pressure for stripping reaction tower 10 can be by adjusting
Temperature and pressure of charging etc. is adjusted and is arranged.
In a preferred embodiment, the third temperature can be set to 20-100 DEG C, and the 4th temperature can be with
It is arranged to 30-90 DEG C, fore-running column overhead temperatures can be set to 100-115 DEG C, and primary distillation tower column bottom temperature can be set
It it is 120-160 DEG C, primary distillation tower tower top pressure can be set to 0-0.03MPa (gauge pressure), and tower bottom pressure can be set to 0-
0.35MPa (gauge pressure).The temperature and pressure of primary distillation tower can by adjusting charging temperature and pressure, boil ratio, reflux ratio again etc. and come
It is adjusted and is arranged.
In a preferred embodiment, stripping 10 bottom of tower of reaction tower is without reboiler, and stripping 10 tower top of reaction tower is without cold
Solidifying reflux.
Fig. 2 diagrammatically illustrates a preferred embodiment according to the present utility model.Wherein, it provides a kind of with containing
The system that the pentose solution of acid continuously prepares furfural, including stripping reaction tower 10, steam (vapor) outlet 11, the first feed(raw material)inlet 12, vapour
Carry steam inlet 13, acid solution outlet 14, separative element 20, ceramic filter 21, cyclone separator 22, lye input port 23 is pure
Change unit 30, fore-running tower reboiler 31, primary distillation tower 32, primary distillation tower feed inlet 33, primary distillation tower steam (vapor) outlet 34, aqueous phase liquid entrance
35, primary distillation tower condenser 36, primary distillation tower liquid separation tank 37, refining plant 38, primary distillation tower bottom liquid outlet 39, heat exchange unit 40,
Second feed(raw material)inlet 41, material outlet 42, furfural entrance 43, furfural outlet 44, furfuryl aldehyde solution heat exchanger 45, acid solution heat exchanger
50, waste water evaporator 60.
The device can continuously prepare furfural with following techniques.
The stripped vapor of second temperature enters from the stripped vapor entrance 13 of 10 bottom of stripping reaction tower in tower, the first temperature
The pentose solution containing acid enter in tower from first feed(raw material)inlet 12 at stripping reaction tower 10 top, the pentose solution containing acid is in vapour
It carries and cyclodehydration reaction generation furfural occurs in reaction tower 10, acid is catalyst, and then, the furfural of generation is anti-from stripping with steam
The steam (vapor) outlet 11 at 10 top of tower is answered to produce, acid solution outlet 14 extraction of the acid solution from 10 bottom of stripping reaction tower.
The steam containing furfural of extraction enter with the separative element 20 that is connected of stripping reaction tower 10, lye is from lye input port 23
Into separative element 20, neutralize the acid in steam containing furfural, then steam enter cyclone separator 22 will neutralize obtained salt with
The steam containing furfural that the isolated acid content of steam containing furfural reduces, the steam containing furfural that acid content reduces continue through ceramic mistake
Filter 21 further removes the impurity in steam, prevents steam from coking and reducing the generation of aldehyde mud in follow-up heat transfer process.
Steam containing furfural enters heat exchange unit 40 by furfural entrance 43, and the pentose solution containing acid passes through the second feed(raw material)inlet
41 enter heat exchange units 40, the pentose solution containing acid and steam containing furfural respectively by material channel and furfural channel, channel it
Between be mutually isolated but can make the pentose solution containing acid and steam containing furfural to carry out heat exchange, after heat exchange containing sour pentose solution
Stripping reaction tower 10 is entered by the first feed(raw material)inlet 12 after the output of material outlet 42, the furfuryl aldehyde solution of gained is from chaff after heat exchange
44 output of aldehyde outlet.
Then, furfuryl aldehyde solution enters the purification unit 30 being connected with separative element 20, and furfuryl aldehyde solution is through furfuryl aldehyde solution first
Heat exchanger 45 is cooled to third temperature, then from primary distillation tower feed inlet 33 enter primary distillation tower 32, in primary distillation tower 32 after purification from
The steam containing furfural of the extraction of primary distillation tower steam (vapor) outlet 34 of tower top after purification, then, steam containing furfural after purification enters fore-running
Tower condenser 36 carries out being cooled to the 4th temperature, is then fed to primary distillation tower liquid separation tank 37, the liquid separation in primary distillation tower liquid separation tank 37
Aqueous phase liquid and oil phase liquid are obtained, aqueous phase liquid is back to by aqueous phase liquid entrance 35 in primary distillation tower 32, and oil phase liquid is defeated
Go out as chaff aldehyde product；A part of bottom liquid of 39 extraction of primary distillation tower bottom liquid outlet exchanges heat through fore-running tower reboiler 31
Become afterwards and boil steam again, returns to primary distillation tower 32 through boiling steam inlet again, rest part bottom liquid is produced as waste water.
In a preferred embodiment, which can also include acid solution heat exchanger 50, for receiving from acid solution
The acid solutions of 14 outflow of mouth simultaneously carry out thermal energy recycling.
In a preferred embodiment, purification unit 30 can also include refining plant 38, for the chaff
Aldehyde product be dehydrated and take off light refined to obtain product furfural.
In a preferred embodiment, which can also include waste water evaporator 60, for a part of fore-running
32 bottom liquid of tower is evaporated recycling.
In a preferred embodiment, first temperature can be set to 80-155 DEG C, the second temperature
It can be set to 150-220 DEG C, stripping 10 tower top temperature of reaction tower can be set to 140-210 DEG C, and column bottom temperature can be with
It is arranged to 150-220 DEG C, stripping 10 tower top pressure of reaction tower can be set to 0.26-2.2MPa (gauge pressure), tower bottom pressure
It can be set to 0.37-2.2MPa (gauge pressure).Strip reaction tower 10 temperature and pressure can by adjusting charging temperature and
Pressure etc. is adjusted and is arranged.
In a preferred embodiment, the third temperature can be set to 20-100 DEG C, and the 4th temperature can be with
It is arranged to 30-90 DEG C, 32 tower top temperature of primary distillation tower can be set to 100-115 DEG C, and column bottom temperature can be set to
120-160℃；32 tower top pressure of primary distillation tower can be set to 0-0.03MPa (gauge pressure), and tower bottom pressure can be set to 0-
0.35MPa (gauge pressure).The temperature and pressure of primary distillation tower 32 can by adjusting charging temperature and pressure, boil ratio and reflux ratio again etc.
To be adjusted and be arranged.
Embodiment
Using system as shown in Figure 2, furfural is continuously prepared with the pentose solution containing acid.
Wherein, using the pentose solution that pentose sugar concentration is 5g/l as pentose material solution, sulfuric acid conduct is added thereto
Catalyst so that the sulfuric acid concentration in pentose solution is 4wt%.This pentose solution containing acid is warming up to via heat exchange unit 40
Enter stripping reaction tower 10 from the first feed(raw material)inlet 12 after 150 DEG C.At the same time, by temperature be 180 DEG C stripped vapor from vapour
Steam inlet 13 is carried to be input in stripping reaction tower 10.The stripped vapor of rising and pentose solution counter current contacting, by pentose solution
170 DEG C are heated to about, cyclodehydration reaction is carried out in reaction tower 10.The furfural of generation enters stripped vapor, with 170 DEG C from vapour
The steam (vapor) outlet 11 for carrying 10 top of reaction tower produces (tower top pressure 0.74MPa), and furfural is contained in the steam containing furfural of extraction
8wt%.
The steam containing furfural of extraction is exported to separative element 20, gas phase neutralization is carried out with 12wt% sodium carbonate liquors, by
Cyclone separator 22 detaches the salt of gained with steam containing furfural, to obtain the steam containing furfural of acid content reduction.Then, should
Steam containing furfural enters ceramic filter 21, enters heat exchange unit 40 after filtering.
In heat exchange unit 40, filtered steam containing furfural is exchanged heat to obtain temperature with the pentose solution containing acid is
170 DEG C of furfuryl aldehyde solution.
Furfuryl aldehyde solution enters purification unit 30.Furfuryl aldehyde solution after furfuryl aldehyde solution heat exchanger 45 further cools to 85 DEG C from
Primary distillation tower feed inlet 33 enters primary distillation tower 32, produces chaff aldehyde steam from primary distillation tower steam (vapor) outlet 34 after purification.It is cold through primary distillation tower
Condenser 36 enters primary distillation tower liquid separation tank 37 after condensing to 80 DEG C, and liquid separation obtains aqueous phase liquid and oil phase liquid, wherein aqueous phase liquid
It is 6wt%, the aqueous 8wt% of oil phase liquid containing aldehyde concentration.
Aqueous phase liquid is returned from 37 top of primary distillation tower liquid separation tank, and enters primary distillation tower 32, oil phase from aqueous phase liquid entrance 35
Liquid output is used as chaff aldehyde product, into chaff aldehyde storage tank.
The chaff aldehyde product through subsequent dehydration, it is de- light refined after can be used as product furfural.Furaldehyde yield is 88% (phase
For the theoretical yield of the pentose solution of 5g/l).
In addition, the temperature containing acid solution of 14 extraction of acid solution outlet of 10 bottom of stripping reaction tower is 175 DEG C, exchange heat through acid solution
Device 50 can cool to 120 DEG C of recyclings after recovering energy.Fore-running tower reboiler 31 is gone out by steam heating, primary distillation tower bottom liquid
A part of bottom liquids of 39 extraction of mouth become after the heat exchange of fore-running tower reboiler 31 boils steam again, is returned through boiling steam inlet again
Primary distillation tower 32, rest part bottom liquid are produced as waste water, and the waste water of extraction can enter waste water evaporator 60, through double evaporation-cooling
After recycle.
The utility model is illustrated by above-described embodiment, but it is to be understood that, above-described embodiment is
Purpose for illustrating and illustrating, and be not intended to limit the invention within the scope of described embodiment.In addition ability
Field technique personnel are it is understood that the utility model is not limited to above-described embodiment, and introduction according to the present utility model is also
More kinds of variants and modifications can be made, these variants and modifications all fall within the utility model range claimed with
It is interior.The scope of protection of the utility model is defined by the appended claims and its equivalent scope.
Claims (14)
1. a kind of with the pentose solution system that continuously prepares furfural containing acid, wherein the system includes：
Strip reaction tower comprising be located at steam (vapor) outlet and first feed(raw material)inlet at top, and the stripped vapor positioned at bottom
Entrance and acid solution outlet；Wherein, first feed(raw material)inlet is used to receive the pentose solution containing acid of the first temperature as raw material
To carry out cyclodehydration reaction, the stripped vapor entrance is used to receive the stripped vapor of second temperature, and the steam (vapor) outlet is used
In providing by the steam containing furfural obtained by the reaction, the acid solution outlet from bottom of tower for producing acid solution；
Separative element is connected with the steam (vapor) outlet, for neutralizing the acid in steam containing furfural, and by the salt of gained and contains chaff
Aldehyde steam detaches, to provide the steam containing furfural of acid content reduction；And
Purification unit is used to purify the furfural of gained.
2. system according to claim 1, wherein the separative element further includes filter device, which is used for
The steam containing furfural reduced to the acid content is filtered, to provide filtered steam containing furfural.
3. system according to claim 1 or 2, wherein the system further includes heat exchange unit comprising：
Material channel, including the second feed(raw material)inlet, the second feed(raw material)inlet are used to receive penta containing acid of the temperature less than the first temperature
Sugar juice；And material outlet, the material outlet are connected with first feed(raw material)inlet, for being carried to the stripping reaction tower
For the pentose solution containing acid of the first temperature, and
Furfural channel is mutually isolated with material channel but can carry out heat exchange, and includes furfural entrance, furfural entrance and institute
It states separative element to be connected, for receiving the steam containing furfural from separative element；It is exported with furfural, furfural outlet and the purifying
Unit is connected, for providing furfuryl aldehyde solution.
4. system according to claim 3, wherein the purification unit includes：
There is primary distillation tower primary distillation tower feed inlet, primary distillation tower steam (vapor) outlet and aqueous phase liquid positioned at top positioned at middle part to enter
Mouth boils steam inlet and the outlet of primary distillation tower bottom liquid again positioned at bottom；
Furfuryl aldehyde solution heat exchanger, furfuryl aldehyde solution are cooled to third temperature through furfuryl aldehyde solution heat exchanger and enter just through primary distillation tower feed inlet
Evaporate tower；
It is furnished with condensation reflux unit equipped with fore-running tower reboiler, tower top in the primary distillation tower bottom of tower；The condensation reflux unit includes
Primary distillation tower condenser and primary distillation tower liquid separation tank；
The fore-running tower reboiler becomes after being used to exchange heat a part of bottom liquid boils steam again, is returned through boiling steam inlet again
Primary distillation tower；
Primary distillation tower condenser is connected with primary distillation tower steam (vapor) outlet, for condensing steam containing furfural after purification to the 4th temperature
The condensate liquid of degree；
Primary distillation tower liquid separation tank, is connected with primary distillation tower condenser, for receiving the condensate liquid, carries out liquid separation to obtain water phase liquid
Body and oil phase liquid, and send the aqueous phase liquid back to primary distillation tower through the aqueous phase liquid entrance, the oil phase liquid is exported
As chaff aldehyde product.
5. system according to claim 1, wherein the separative element, which includes lye input port, to be used for to input lye
With the acid in steam containing furfural.
6. system according to claim 1, wherein the separative element includes cyclone separator, for by the salt with
Steam containing furfural detaches, to provide the steam containing furfural of acid content reduction.
7. system according to claim 1, wherein the system also includes acid solution heat exchangers, for receiving from the acid
The acid solution of liquid outlet outflow simultaneously carries out thermal energy recycling.
8. system according to claim 4, wherein the purification unit further includes refining plant, for the chaff
Aldehyde product be dehydrated and take off light refined to obtain product furfural.
9. system according to claim 4, wherein the system also includes waste water evaporator, the waste water evaporator with
The outlet of primary distillation tower bottom liquid is connected, for being evaporated to another part bottom liquid exported from primary distillation tower bottom liquid
It recycles.
10. system according to claim 1, wherein first temperature can be arranged to 80-155 DEG C, and described second
Temperature can be arranged to 150-220 DEG C, and stripping reaction column overhead temperatures can be arranged to 140-210 DEG C, strip reaction tower
Column bottom temperature can be arranged to 150-220 DEG C.
11. system according to claim 1, wherein in terms of gauge pressure, the stripping reaction tower tower top pressure can be set
For 0.26-2.2MPa, stripping reaction tower tower bottom pressure can be arranged to 0.37-2.2MPa.
12. system according to claim 4, wherein the third temperature can be arranged to 20-100 DEG C, the 4th temperature
It can be arranged to 30-90 DEG C, fore-running column overhead temperatures can be arranged to 100-115 DEG C, and primary distillation tower column bottom temperature can be by
It is set as 120-160 DEG C.
13. system according to claim 4, wherein in terms of gauge pressure, the primary distillation tower tower top pressure can be arranged to 0-
0.03MPa, tower bottom pressure can be arranged to 0-0.35MPa.
14. system according to claim 1, wherein the stripping reaction tower bottom of tower is without reboiler, stripping reaction column overhead
Frozen-free reflux.
Priority Applications (10)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721684194.7U CN208055237U (en) | 2017-12-06 | 2017-12-06 | The system for continuously preparing furfural with the pentose solution containing acid |
| CA3083403A CA3083403A1 (en) | 2017-12-06 | 2018-11-27 | System and method for continuously preparing furfural using acid-containing pentose solution |
| DK18885810.4T DK3722288T3 (en) | 2017-12-06 | 2018-11-27 | System and method for continuous production of furfural using acidic pentose solution |
| EP18885810.4A EP3722288B1 (en) | 2017-12-06 | 2018-11-27 | System and method for continuously preparing furfural using acid-containing pentose solution |
| FIEP18885810.4T FI3722288T3 (en) | 2017-12-06 | 2018-11-27 | System and method for continuously preparing furfural using acid-containing pentose solution |
| PL18885810.4T PL3722288T3 (en) | 2017-12-06 | 2018-11-27 | System and method for continuously preparing furfural using acid-containing pentose solution |
| PT188858104T PT3722288T (en) | 2017-12-06 | 2018-11-27 | System and method for continuously preparing furfural using acid-containing pentose solution |
| PCT/CN2018/117648 WO2019109834A1 (en) | 2017-12-06 | 2018-11-27 | System and method for continuously preparing furfural using acid-containing pentose solution |
| ES18885810T ES2981778T3 (en) | 2017-12-06 | 2018-11-27 | System and method for preparing furfural continuously using a pentose solution containing acid |
| US16/894,564 US11142510B2 (en) | 2017-12-06 | 2020-06-05 | System and method for continuously preparing furfural using acid-containing pentose solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721684194.7U CN208055237U (en) | 2017-12-06 | 2017-12-06 | The system for continuously preparing furfural with the pentose solution containing acid |
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| Publication Number | Publication Date |
|---|---|
| CN208055237U true CN208055237U (en) | 2018-11-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201721684194.7U Active CN208055237U (en) | 2017-12-06 | 2017-12-06 | The system for continuously preparing furfural with the pentose solution containing acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019109834A1 (en) * | 2017-12-06 | 2019-06-13 | 易高环保能源研究院有限公司 | System and method for continuously preparing furfural using acid-containing pentose solution |
-
2017
- 2017-12-06 CN CN201721684194.7U patent/CN208055237U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019109834A1 (en) * | 2017-12-06 | 2019-06-13 | 易高环保能源研究院有限公司 | System and method for continuously preparing furfural using acid-containing pentose solution |
| US11142510B2 (en) | 2017-12-06 | 2021-10-12 | Eco Environmental Energy Research Institute Limited | System and method for continuously preparing furfural using acid-containing pentose solution |
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