CN109821266A - A kind of furfural multiple-effect reaction and rectification device and technique - Google Patents
A kind of furfural multiple-effect reaction and rectification device and technique Download PDFInfo
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- CN109821266A CN109821266A CN201910206513.0A CN201910206513A CN109821266A CN 109821266 A CN109821266 A CN 109821266A CN 201910206513 A CN201910206513 A CN 201910206513A CN 109821266 A CN109821266 A CN 109821266A
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Abstract
The present invention relates to a kind of furfural multiple-effect reaction and rectification device and techniques, the equipment that this technique uses includes an effect rectifying column and two effect rectifying columns, the tower bottom of one effect rectifying column is provided with effect coupling reboiler, the tower top of one effect rectifying column is disposed with an effect first-stage condenser and an effect secondary coolers, the tower bottom of two effect rectifying columns is provided with two effect reboilers, the tower top of two effect rectifying columns is disposed with two effect first-stage condensers and two effect secondary coolers, the tower bottom of one effect rectifying column is connected to the tower top of two effect rectifying columns by pump, two effect first-stage condensers pass through piping connection to an effect coupling reboiler, two effect reboilers connect external steam import.The design of the invention is scientific and reasonable, and vapor consumption can be greatly reduced, reduce the dosage and power consumption of cooling water, and can be improved rectifying purity, improve furaldehyde yield.
Description
Technical field
The invention belongs to chemical materials reaction rectification technique fields, are related to furfural rectifier unit, in particular to a kind of furfural
Multiple-effect reaction and rectification device and technique.
Background technique
Furfural is widely used, is the Organic Chemicals on basis, and it is the hydrogen on 2, furans that scientific name, which is furaldehyde,
The derivative that atom is replaced by aldehyde radical.It is initially made by rice bran and diluted acid heat together, so being called furfural.Furfural is by pentosan
Hydrolysis generates pentose under the action of an acid, then is cyclized by dehydration of pentoses.The primary raw material of production is the agricultural and sideline productions such as corncob
Product.Furfural is the most important derivative of furans ring system, and chemical property is active, can by aoxidize, be condensed etc. reactions produce it is numerous
Derivative, be widely used in the industry such as synthetic plastic, medicine, pesticide.
Rectifying is the carry out part multiple simultaneously in rectifying column by the mixed liquor as composed by volatility different component
Vaporization and partial condensation, separate it into the process of almost pure state component.
Material becomes steam after reboiler heats and rises in rectifying column in rectifying tower reactor, the phegma on every layer of column plate
Body is contacted with each other with upflowing vapor, carries out the transmittance process of heat and matter.Since there are temperature difference and concentration difference, gas phases on column plate
Partial condensation will be carried out, is transferred to part of difficult volatile component in liquid phase；And the latent heat that vapor condensation releases is transmitted to liquid
Phase vaporizes liquid phase part, and part of volatile components are transferred in gas phase.The long and causes the liquid phase for leaving this layer of column plate
It is low when the concentration of middle volatile components is compared with the entrance plate, and the height that volatile components concentration relatively enters in the gas phase left.
If gas-liquid two-phase onboard time of contact long enough, then the gas-liquid two-phase for leaving the plate is mutually balance.Every laminate of rectifying column
On all carry out above-mentioned similar process.
In chemical industry, distillation process is one of energy consumption maximum unit operation, since global energy has occurred
Since source problem, the power saving of distillation process has caused the attention of people extensively.The energy conservation of distillation process substantially can be with
Set about from following several respects: (1) distillation process thermal energy makes full use of；(2) distillation process itself is reduced to the needs of energy；
(3) thermodynamic efficiency of distillation system is improved；(4) using qualified separation system.
Under normal conditions, it reacts and separates two kinds of operations and usually carried out in the individual equipment of two classes respectively.If can be by two
Person combines, and carries out simultaneously within one device, and product or intermediate product that reaction generates are separated in time, then can be improved
The yield of product, while being separated again using reaction heat for product, reach energy-efficient purpose.
Multi-effect distillation is to provide heat to the reboiler of lower pressure column using high pressure tower top latent heat of the steam to be thermally integrated rectifying
System.Compared with single column, multi-effect distillation can greatly improve the utilization rate of energy, largely save rectifier unit
Energy consumption, and the product quality of rectifying is higher than the quality of single-action rectifying, yield also improves.
Furfural production process mainly includes one-step method and two-step method, the one-step method used in industrial production at present, furfural receipts
Rate is low, general only 50% or so and seriously polluted.Two-step method is exactly by hydrolysis of hemicellulose reaction and dehydration of pentoses into chaff
The reaction of aldehyde is separated into two independent steps and carries out.When being pre-processed to biomass, since hemicellulose is noncrystalline knot
Structure, the degree of polymerization are low, degree of branching is high, pentose can be dissolved and are hydrolyzed into cell wall under suitable pretreatment condition, be rich in
Catalysis reaction produces furfural under the hydrolyzate acid condition of pentose.Two-step method is due to target product independence in two reactors
So that reaction process by-product is less, furfural yield is relatively high.
The multi-effect distillation of the furfural energy saving technique emerging as one, it mainly with low energy consumption, low-grade energy utilize and
Efficient thermodynamic efficiency causes the great attention of people.The multiple-effect reactive distillation one of furfural imitate rectifying column be the first pressurizing tower,
Two effect rectifying columns are the second pressurizing tower, and this multiple-effect reactive distillation can greatly reduce energy consumption, improve the yield of furfural.
By the retrieval to patent document, patent document identical with present patent application is not found.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide one kind can be greatly reduced vapor consumption,
The dosage and power consumption for reducing cooling water, improve the furfural multiple-effect reaction and rectification device and technique of furaldehyde yield.
The present invention solves its technical problem and is achieved through the following technical solutions:
A kind of furfural multiple-effect reaction and rectification device, it is characterised in that: including one effect rectifying column and two effect rectifying columns, described one
The tower bottom of effect rectifying column is provided with effect coupling reboiler, and the tower top of the effect rectifying column is disposed with effect level-one condensation
Device and an effect secondary coolers, the tower bottom of the two effects rectifying column are provided with two effect reboilers, the tower top of the two effects rectifying column
Two effect first-stage condensers and two effect secondary coolers are disposed with, the tower bottom of the effect rectifying column is connected to described by pump
The tower top of two effect rectifying columns, the two effect first-stage condenser pass through piping connection to the effect coupling reboiler, two effect
Reboiler connects external steam import.
Moreover, further including feed exchanger, the tower bottom of described effect the top of the distillation column and the two effects rectifying column passes through
Piping connection is to the feed exchanger.
Moreover, the two effect first-stage condenser passes through piping connection to the effect rectifying column.
Moreover, the external steam import passes through piping connection to the two effects rectifying column.
A kind of technique of furfural multiple-effect reactive distillation, characterized by the following steps:
1) raw material of pentose solution containing catalyst preheated in feed preheater by be located at one effect the top of the distillation column into
Material mouth enters in an effect rectifying column；
2) material at an effect rectifying tower bottom is by an effect coupling reboiler or external steam heating and gasifying, by tower reactor
After Mass and heat transfer, steam rises to tower top and condenses；
3) steam in an effect rectifying column is condensed by an effect first-stage condenser of an effect the top of the distillation column, and condensate liquid enters
One effect secondary coolers after cool to 50 DEG C hereinafter, coolant liquid a part containing furfural be back to an effect rectifying column and with it is upper
The steam risen carries out Mass and heat transfer, forms stable temperature and concentration gradient, and another part extraction enters furfural treatment workshop section；
4) raw material that unreacted pentose solution imitates rectifying columns as two in an effect rectifying tower bottom enters two via pump
The top of the distillation column is imitated, is heated by two effect reboilers or external steam, steam rises to two effect the top of the distillation column, Jing Erxiao mono-
Grade condenser condensation, two effect secondary coolers simultaneously cool to 50 DEG C hereinafter, being partly refluxed to two effect rectifying columns, and another part produces
Into furfural treatment workshop section；
5) the unreacted material in two effect rectifying tower bottoms and material liquid exchange heat in feed exchanger and enter hydrolysis work
Section.
Moreover, the mass fraction of pentose is 4%~15% in the pentose solution.
Moreover, the catalyst be sulfuric acid and or formic acid and or acetic acid and or strong acid weak base salt and or nitric acid.
Moreover, the effect coupling reboiler and the steam pressure of two effect first-stage condensers are 0.4~0.8MPa, it is described
The steam pressure of two effect reboilers is 0.6~1.5MPa, and the steam pressure of the effect first-stage condenser is 0.3~0.7MPa.
The advantages and benefits of the present invention are:
1, the steam of furfural multiple-effect reactive distillation of the invention, an effect rectifying column can be directly logical by two effect first-stage condensers
Enter tower body, it is passed through tower body again after can also pass through effect coupling reboiler；External steam can be passed directly into two effect rectifying columns,
It can determine that steam inlet can with specific reference to the quantity of steam in multi-effect distillation device by being passed through tower body again after two effect reboilers
Flexibly control.
2, furfural multiple-effect reactive distillation of the invention increases feed exchanger, is able to ascend the entrance temperature of material, saves
Rectifying steam consumption.
3, furfural multiple-effect reactive distillation of the invention can be improved rectifying purity, improve furaldehyde yield, furaldehyde yield can
Reach 75% or more.
4, vapor consumption can not only be greatly reduced compared with conventional distillation in furfural multiple-effect reactive distillation of the invention
Amount reduces the dosage and power consumption of cooling water, improves thermodynamic efficiency, so that distillation process thermal energy can make full use of, reduces
Distillation process itself is computed the needs of energy, and one ton of furfural of every production can save about 8 tons of steam consumption.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Description of symbols
It is cold that 1- mono- imitates rectifying column, 2- bis- imitates rectifying column, 3- feed exchanger, 4- bis- imitate first-stage condenser, 5- bis- imitates second level
But device, 6- bis- imitate reboiler, 7- pump, 8- mono- and imitate first-stage condenser, the effect of 9- mono- secondary coolers, the effect coupling reboiler of 10- mono-.
Specific embodiment
Below by specific embodiment, the invention will be further described, and it is not limit that following embodiment, which is descriptive,
Qualitatively, this does not limit the scope of protection of the present invention.
As shown, present embodiment uses fair current process, it is specific as follows:
A kind of furfural multiple-effect reaction and rectification device, including an effect rectifying column 1 and two effect rectifying columns 2, the tower of an effect rectifying column
Bottom is provided with effect coupling reboiler 10, and the tower top of an effect rectifying column is disposed with an effect first-stage condenser 8 and an effect second level
Cooler 9, the tower bottom of two effect rectifying columns are provided with two effect reboilers 6, and the tower top of two effect rectifying columns is disposed with two effect level-ones
Condenser 4 and two effect secondary coolers 5, the tower bottom of an effect rectifying column are connected to the tower top of two effect rectifying columns, an effect essence by pump
The tower top for evaporating tower leads to pentose solution, the tower bottom liquid that two effect the top of the distillation column are come in from an effect rectifying column, an effect of an effect rectifying column
Reboiler is coupled by piping connection to two effect first-stage condensers, the two effect reboilers at two effect rectifying tower bottoms connect external steam
Import.
Further include feed exchanger 3, the tower bottom of an effect the top of the distillation column and two effect rectifying columns pass through piping connection into
Expect heat exchanger.
Pentose solution mass fraction into an effect the top of the distillation column is 10%, and the mass fraction of catalyst sulfuric acid is
0.5%, while also containing a small amount of furfural, mass fraction 0.7%, remaining ingredient is water, mass fraction 88.7%.Pentose is molten
Liquid temperature is 90 DEG C, and an effect the top of the distillation column, feed rate 10000kg/h are entered after feed exchanger is preheating to 140 DEG C.
The feed pressure of one effect rectifying column is 0.5MPa, and theoretical cam curve is 10 pieces, tower top pressure 0.4MPa, pressure drop 5kPa, one
Effect rectifying column heats in such a way that steam is directly entered tower bottom, and heating steam is 160 DEG C, steam pressure 0.52MPa, wherein
Steam is heated from two effect the top of the distillation column condensers, steam flow 3100kg/h, effect the top of the distillation column temperature is 151.9
DEG C, column bottom temperature is 152.5 DEG C, and after Jing Yixiao distillation column reactor, pentose is partially converted into furfural under the effect of the catalyst.
The furfural overwhelming majority generated in an effect rectifying column is produced in the form of furfural aqueous solution from tower top, is entered later
Furfural treatment workshop section, it is 357.9kg/h that furfural, which produces mass flow,.Tower bottom produces aqueous solution after an effect distillation column reactor rectifying
22.8kg/h containing furfural (mass fraction 0.3%), pentose 514.4kg/h (mass fraction 6%), an effect rectifying column materials at bottom of tower warp
Pump enters two effect rectifying columns.
Two effect 2 theoretical cam curves of rectifying column are 10 pieces, tower top pressure 0.7MPa, full tower pressure drop 5kPa, tower top temperature 170.2
DEG C, column bottom temperature is 170.5 DEG C.Two effect rectifying columns are directly heated by external saturated steam, and vapor (steam) temperature is 175.1 DEG C, pressure
Power is 0.8MPa, and the flow of steam is 3000kg/h.Remaining pentose overwhelming majority in two effect rectifying columns is converted into furfural, furfural
It is produced in the form of furfural aqueous solution from two effect the top of the distillation column, enters furfural treatment workshop section later, furfural produces mass flow
For 298.4kg/h.The remaining aqueous solution containing a small amount of furfural (mass fraction 0.2%) and pentose (mass fraction 0.9%) into
Enter to feed preheater, hydrolysis workshop section is returned after feed exchanger.
Operating process of the invention are as follows:
1) raw material of pentose solution containing catalyst preheated in feed preheater by be located at one effect the top of the distillation column into
Material mouth enters in an effect rectifying column；
2) material at an effect rectifying tower bottom is by an effect coupling reboiler or external steam heating and gasifying, by tower reactor
After Mass and heat transfer, steam rises to tower top and condenses；
3) steam in an effect rectifying column is condensed by an effect first-stage condenser of an effect the top of the distillation column, and condensate liquid enters
One effect secondary coolers after cool to 50 DEG C hereinafter, coolant liquid a part containing furfural be back to an effect rectifying column and with it is upper
The steam risen carries out Mass and heat transfer, forms stable temperature and concentration gradient, and another part extraction enters furfural treatment workshop section；
4) raw material that unreacted pentose solution imitates rectifying columns as two in an effect rectifying tower bottom enters two via pump
The top of the distillation column is imitated, is heated by two effect reboilers or external steam, steam rises to two effect the top of the distillation column, Jing Erxiao mono-
Grade condenser condensation, two effect secondary coolers simultaneously cool to 50 DEG C hereinafter, being partly refluxed to two effect rectifying columns, and another part produces
Into furfural treatment workshop section；
5) the unreacted material in two effect rectifying tower bottoms and material liquid exchange heat in feed exchanger and enter hydrolysis workshop section.
Although disclosing the embodiment of the present invention and attached drawing for the purpose of illustration, those skilled in the art can be managed
Solution: do not departing from the present invention and spirit and scope of the appended claims in, various substitutions, changes and modifications be all it is possible,
Therefore, the scope of the present invention is not limited to the embodiment and attached drawing disclosure of that.
Claims (8)
1. a kind of furfural multiple-effect reaction and rectification device, it is characterised in that: including an effect rectifying column and two effect rectifying columns, an effect
The tower bottom of rectifying column is provided with effect coupling reboiler, and the tower top of the effect rectifying column is disposed with an effect first-stage condenser
And effect secondary coolers, the tower bottom of the two effects rectifying column are provided with two effect reboilers, the tower top of the two effects rectifying column according to
Secondary to be provided with two effect first-stage condensers and two effect secondary coolers, the tower bottom of the effect rectifying column is connected to described two by pump
The tower top of rectifying column is imitated, the two effect first-stage condenser is by piping connection to the effect coupling reboiler, and two effect is again
It boils device and connects external steam import.
2. furfural multiple-effect reaction and rectification device according to claim 1, it is characterised in that: it further include feed exchanger, institute
The tower bottom for stating an effect the top of the distillation column and the two effects rectifying column passes through piping connection to the feed exchanger.
3. furfural multiple-effect reaction and rectification device according to claim 1, it is characterised in that: the two effects first-stage condenser is logical
Piping connection is crossed to the effect rectifying column.
4. furfural multiple-effect reaction and rectification device according to claim 1, it is characterised in that: the external steam import passes through
Piping connection to it is described two effect rectifying column.
5. furfural multiple-effect reaction and rectification device according to claim 1, it is characterised in that: it is described one effect coupling reboiler and
Two effect first-stage condensers steam pressures be 0.4~0.8MPa, it is described two effect reboiler steam pressure be 0.6~
The steam pressure of 1.5MPa, the effect first-stage condenser are 0.3~0.7MPa.
6. a kind of technique of furfural multiple-effect reactive distillation, characterized by the following steps:
1) raw material of pentose solution containing catalyst preheated in feed preheater is by being located at a feed inlet for imitating the top of the distillation column
It enters in an effect rectifying column；
2) material at an effect rectifying tower bottom is by an effect coupling reboiler or external steam heating and gasifying, by the caloic in tower reactor
After transmitting, steam rises to tower top and condenses；
3) steam in an effect rectifying column is condensed by an effect first-stage condenser of an effect the top of the distillation column, and condensate liquid enters an effect
Cooled after secondary coolers to 50 DEG C hereinafter, coolant liquid a part containing furfural be back to an effect rectifying column and with rising
Steam carries out Mass and heat transfer, forms stable temperature and concentration gradient, and another part extraction enters furfural treatment workshop section；
4) raw material that unreacted pentose solution imitates rectifying columns as two in an effect rectifying tower bottom enters two effects essence via pump
Column overhead is evaporated, is heated by two effect reboilers or external steam, steam rises to two effect the top of the distillation column, and Jing Erxiao level-one is cold
Condenser condensation, two effect secondary coolers simultaneously cool to 50 DEG C hereinafter, being partly refluxed to two effect rectifying columns, and another part extraction enters
Furfural treatment workshop section；
5) the unreacted material in two effect rectifying tower bottoms and material liquid exchange heat in feed exchanger and enter hydrolysis workshop section.
7. furfural multiple-effect reactive distillation process according to claim 6, it is characterised in that: pentose in the pentose solution
Mass fraction be 4%~15%.
8. furfural multiple-effect reactive distillation process according to claim 6, it is characterised in that: the catalyst be sulfuric acid and
Or formic acid and or acetic acid and or strong acid weak base salt and or nitric acid.
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| CN201910206513.0A CN109821266A (en) | 2019-03-19 | 2019-03-19 | A kind of furfural multiple-effect reaction and rectification device and technique |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112902686A (en) * | 2021-01-26 | 2021-06-04 | 河北易高生物能源有限公司 | Furfural primary distillation tower steam recycling method |
| CN113666893A (en) * | 2021-09-23 | 2021-11-19 | 中国矿业大学(北京) | Refining method of furfural |
| CN114225453A (en) * | 2021-11-26 | 2022-03-25 | 安徽金禾实业股份有限公司 | Device and method for extracting furfuryl alcohol by rectification in maltol production |
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| CN112902686A (en) * | 2021-01-26 | 2021-06-04 | 河北易高生物能源有限公司 | Furfural primary distillation tower steam recycling method |
| CN113666893A (en) * | 2021-09-23 | 2021-11-19 | 中国矿业大学(北京) | Refining method of furfural |
| CN114225453A (en) * | 2021-11-26 | 2022-03-25 | 安徽金禾实业股份有限公司 | Device and method for extracting furfuryl alcohol by rectification in maltol production |
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