CN105461669B - A kind of refined furfural dehydration deacidifying device and process for refining - Google Patents
A kind of refined furfural dehydration deacidifying device and process for refining Download PDFInfo
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- CN105461669B CN105461669B CN201510995139.9A CN201510995139A CN105461669B CN 105461669 B CN105461669 B CN 105461669B CN 201510995139 A CN201510995139 A CN 201510995139A CN 105461669 B CN105461669 B CN 105461669B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
- C07D307/48—Furfural
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Abstract
The invention belongs to chemicals furfural production technology technical fields, it is not thorough to solve dehydration depickling in existing furfural production, in be dehydrated deacidification aldehyde is taken away simultaneously, lead to problems such as to cause waste, increase facility load, a kind of refined furfural is provided and is dehydrated deacidifying device and process for refining.Hair aldehyde, which enters in dehydration extracting tower, to react, and acid liquid phase transformation vapour phase runs up recycling, and aldehyde becomes liquid phase and flows downwardly into treating column, and condensing recovery finished product aldehyde in treating column, residue is discharged；Sour water, which enters condenser, becomes liquid phase, and partial reflux, which enters, is dehydrated extracting tower, and part flows into layering tank layering, and thick aldehyde tank is recovered into after aldehyde is static, and thick aldehyde original fluid container is added by de- light bottom portion in sour water, is flowed into light component tank after organic impurities is condensed.The acid of thick aldehyde has carried out complete recycling, and the rate of recovery of smart aldehyde improves 3%-5% than of the same trade, and the purity of furfural is increased to 99.5% or more, and the stable quality of smart aldehyde disclosure satisfy that the demand of market high-end user to top grade product.
Description
Technical field
The invention belongs to chemicals furfural production technology technical fields, and in particular to a kind of refined furfural dehydration depickling dress
It sets and process for refining.
Background technology
Two kinds of the current furfural production in China are dehydrated acid stripping methods：With soda ash neutralisation：Sulfuric acid is neutralized to neutrality, then
It is dehydrated with the way of distillation；Method is washed with water：It is dissolved in characteristic of the water insoluble in aldehyde using sulfuric acid, dilutes the acid in furfural with a large amount of clear water,
Achieve the effect that depickling.
Both the above acid stripping method all has a significant impact to the furfural rate of recovery, and first method makes furfural tree in subtractive process
Esterification, forms aldehyde mud, and the rate of recovery is low；Second method uses a large amount of clear water, and no less than 3% is taken away while being dehydrated depickling
Aldehyde, can not recycle, while depickling water causes the loss and waste of heat by the evaporation of waste water evaporator, both increases equipment
Burden, is also unfavorable for energy-saving.
Soda ash neutralisation, furfural itself or the organic side reaction occurred with other substances in solution under the conditions of causing.It causes
The generation of unknown substance.To cause the loss of furfural.Influence the purity of the rate of recovery and furfural of furfural.
And WATER-WASHING METHOD is to be dissolved in characteristic of the water insoluble in aldehyde using acid, dilutes thick aldehyde with a large amount of softening clear water（10%
Water, 90% aldehyde）Interior acid takes water, the acid of thick aldehyde out of with water, achievees the effect that depickling.This kind of a large amount of softening of method waste is clear
Water, 1 ton of thick aldehyde need to use 0.3-0.5 tons of water.Thick aldehyde is lost, the aldehyde not less than 3% has been taken away in clear water.It is to pass through steaming to handle aldehyde water
Vapour heats, and needs to waste thermal energy.
Invention content
The present invention is not thorough to solve dehydration depickling in existing furfural production, while being taken away in being dehydrated deacidification
Aldehyde leads to cause waste, increases facility load, provides a kind of refined furfural dehydration deacidifying device and process for refining.
The present invention is realized by following technical solution：A kind of refined furfural dehydration deacidifying device, includes equipped with liquid level gauge
Thick aldehyde original fluid container, the liquid outlet of thick aldehyde original fluid container is pumped by hair aldehyde to be connect with high-order storage tank, and the liquid outlet connection of high-order storage tank is de-
Inlet in the middle part of water extracting tower, dehydration depickling tower bottom are connect with treating column, and condenser I, condenser I are installed at the top for the treatment of column
Liquid outlet connect finished product aldehyde tank, the slag notch of condenser I connects raffinate kettle, and raffinate liquid from reactor mouth connects thick aldehyde original fluid container；It is de-
Liquid distribution trough is installed at the top of water extracting tower, condenser II is installed on liquid distribution trough top, and the liquid outlet of condenser II passes through gas
Liquid/gas separator connection layering tank and liquid distribution trough, the outlet connection of layering tank upper liquid take off light system, are layered pot bottom liquid
Outlet connects thick aldehyde tank by static tank, and the de- light system is the de- light kettle that top is connected with condenser III, takes off light bottom portion
Thick aldehyde original fluid container is connected, the liquid outlet of condenser III connects light component tank.
The height of the dehydration extracting tower is 11.3m, and the height of conversion zone is 10.01m, and the inlet for being dehydrated extracting tower is set
At conversion zone 6-7m；It is dehydrated in extracting tower and 3 sections of fillers is set, every section of 3m, the filler is perforated plate corrugated filler, and parameter is：
450Y/∅698。
The finished product aldehyde tank and gas-liquid separator are connected separately with vacuum tank, install vacuum pump at the top of vacuum tank, bottom is set
There is sewage draining exit.The bottom of the dehydration extracting tower, treating column and de- light kettle is equipped with steam heater.
The technique that furfural is refined using the refined furfural dehydration deacidifying device, the specific steps are：Thick aldehyde is pumped by hair aldehyde
High-order storage tank is pumped into from thick aldehyde original fluid container, the hair aldehyde in high-order storage tank, which enters in the middle part of dehydration extracting tower, to be reacted, sour water
Solution becomes vapour phase by liquid phase, runs up recycling, and aldehyde becomes liquid phase and runs down；Aldehyde liquid is distributed to bottom of tower and flows into treating column,
It is further condensed back in treating column in income finished product aldehyde tank, residue is discharged into raffinate kettle, and residue is discharged raffinate kettle, and liquid is condensed back to
It takes in thick aldehyde original fluid container；Aqueous acid becomes further being condensed into liquid phase into condenser after gas phase, and aqueous acid passes through gas
Liquid/gas separator passes back into layering tank, and after being layered in layering tank, sour water, which enters, takes off light system, and aldehyde returns after static tank is static
Thick aldehyde tank is taken in, the sour water in de- light system detaches in taking off light kettle, and aqueous acid is added as liquid phase by de- light bottom portion thick
Aldehyde original fluid container, organic impurities flow into after condensation in light component tank as gas phase light component.
The column bottom temperature of the dehydration extracting tower is 130-135 DEG C, and tower top temperature is 70-80 DEG C；The bottom of tower temperature for the treatment of column
Degree is 135-140 DEG C, and tower top temperature is 100-104 DEG C；The de- light kettle bottom temperature is 98-102 DEG C, and kettle top temperature is 86-
90℃.The light component of de- light system removing is the organic impurities such as a small amount of formaldehyde, acetone；Vacuum tank is to vacuumize surge tank, is made
Whole system is in negative pressure state.
The characteristic of water is dissolved in insoluble in aldehyde using acid, after thick aldehyde is pumped into dehydration extracting tower, is dehydrated the bottom of tower of extracting tower
Temperature control is 130-135 DEG C, and tower top temperature control is 70-80 DEG C, and sour water becomes gas phase and runs up at this time, and aldehyde is liquid phase
It is scattered in bottom of tower downwards, since the tower body height of dehydration extracting tower increases, conversion zone is increased, accordingly increases the reflux of sour water
Amount, reduces the dosage of water so that gas-liquid phase separation is thorough, from the middle part feeding of dehydration extracting tower, is conducive to point of sour water and aldehyde
From being carried out at the same time to reach dehydration depickling, the places dehydration extracting tower 8-10m are equipped with filler, that is to say, that filler is installed in anti-
It answers section, filler to be changed to perforated plate corrugated filler by original float valve tray, further enhances the filterability in tower, so that sour
Water and aldehyde thoroughly detach.
Liquid branch device is installed at the top of dehydration extracting tower, increases reflux, regurgitant volume is increased to 100-200kg, is conducive to
The sour water taken off is passed back into again in dehydration extracting tower, and a small amount of sour water left in furfural is made to be further backing out.Sour water becomes
To be further recovered by condenser after gas phase in the static tank of layering, reduce waste, sour water circulating repetition of the present invention carries out
It is dehydrated depickling reaction, wherein no less than 3% aldehyde also recycles simultaneously, reduces the loss of aldehyde, reduces facility load, energy saving drop
Consumption.
The present invention is dissolved in the characteristic of water using acid insoluble in aldehyde, and dehydration depickling is synchronized and is carried out；It is filled out using perforated plate corrugated
Material reinforces filterability；The tower body height of dehydration extracting tower increases, and increases conversion zone, has accordingly increased the regurgitant volume of sour water,
From the middle part feeding of dehydration extracting tower recycling is run up conducive to making sour water become vapour phase from liquid phase；And aldehyde still be liquid phase to
Lower operation is carried out at the same time convenient for detaching sour water and aldehyde to reach dehydration depickling.It is installed at the top of dehydration extracting tower
Liquid branch device, increases reflux, is passed back into again conducive to the sour water taken off in dehydration extracting tower, makes to leave in furfural
A small amount of sour water is further backing out.
The present invention is run by test of many times, and after testing, the acid of thick aldehyde has carried out complete recycling, and the rate of recovery ratio of smart aldehyde is same
Industry improves 3%-5%, and the purity of furfural is increased to 99.5% or more, and the stable quality of smart aldehyde disclosure satisfy that market height to top grade product
The demand of end subscriber.
Description of the drawings
Fig. 1 is that refined furfural of the present invention is dehydrated deacidifying device structural schematic diagram, and Fig. 2 is technological process of the present invention
Figure.
In figure：1- liquid level gauges；The thick aldehyde original fluid containers of 2-；3- maos of aldehyde pumps；4- high position storage tanks；5- is dehydrated extracting tower；5.1- feed liquor
Mouthful；6- treating columns；7- condensers I；8- finished product aldehyde tanks；9- raffinate kettles；10- liquid distribution troughs；11- condensers II；12- gas-liquids point
From device；13- is layered tank；The static tanks of 14-；The thick aldehyde tanks of 15-；16- condensers III；17- takes off light kettle；18- light component tanks.
Specific implementation mode
A kind of refined furfural dehydration deacidifying device, includes the thick aldehyde original fluid container 2 equipped with liquid level gauge 1, thick aldehyde original fluid container 2 goes out
Liquid mouth is connect by hair aldehyde pump 3 with high-order storage tank 4, the inlet at 5 middle part of liquid outlet connection dehydration extracting tower of high-order storage tank 4
5.1,5 bottom of dehydration extracting tower is connect with treating column 6, and condenser I 7 is installed at 6 top for the treatment of column, and the liquid outlet of condenser I 7 connects
It is connected into product aldehyde tank 8, the slag notch connection raffinate kettle 9 of condenser I 7,9 liquid outlet of raffinate kettle connects thick aldehyde original fluid container 2；Dehydration is de-
Liquid distribution trough 10 is installed at 5 top of acid tower, and condenser II 11 is installed on 10 top of liquid distribution trough, and condenser II's 11 goes out liquid
Mouth connects layering tank 13 and liquid distribution trough 10 by gas-liquid separator 12, and the outlet of layering 13 upper liquid of tank connects de- imprisons for light crime
System, layering 13 bottom liquid outlet of tank connect thick aldehyde tank 15 by static tank 14, and the de- light system is that top is connected with condensation
The de- light kettle 17 of device III 16 takes off 17 bottom of light kettle and connects thick aldehyde original fluid container 2, and the liquid outlet of condenser III 16 connects light component
Tank 18.
The height of the dehydration extracting tower is 11.3m, and the height of conversion zone is 10.01m, is dehydrated the inlet of extracting tower
5.1 are set at conversion zone 6-7m；It is dehydrated in extracting tower and 3 sections of fillers is set, every section of 3m, the filler is perforated plate corrugated filler, ginseng
Number is：450Y/∅698.The finished product aldehyde tank 8 and gas-liquid separator 12 are connected separately with vacuum tank, and vacuum is installed at the top of vacuum tank
Pump, bottom are equipped with sewage draining exit.The bottom of the dehydration extracting tower, treating column and de- light kettle is equipped with steam heater.
The technique that furfural is refined using the refined furfural dehydration deacidifying device, the specific steps are：Thick aldehyde passes through hair aldehyde
Pump is pumped into high-order storage tank from thick aldehyde original fluid container, and the hair aldehyde in high-order storage tank, which enters in the middle part of dehydration extracting tower, to be reacted, acid
Aqueous solution becomes vapour phase by liquid phase, runs up recycling, and aldehyde becomes liquid phase and runs down；Aldehyde liquid is distributed to bottom of tower and flows into treating column,
It is further condensed back in treating column in income finished product aldehyde tank, residue is discharged into raffinate kettle, and residue is discharged raffinate kettle, liquid condensation
It is recovered into thick aldehyde original fluid container；Aqueous acid becomes further being condensed into liquid phase into condenser after gas phase, and aqueous acid passes through
Gas-liquid separator, partial reflux enter to be dehydrated extracting tower that the reaction was continued, and part flows into layering tank, after being layered in layering tank, sour water
Into de- light system, aldehyde is recovered into thick aldehyde tank after static tank is static, and the sour water in de- light system detaches in taking off light kettle, acid
Thick aldehyde original fluid container is added by de- light bottom portion as liquid phase in aqueous solution, and organic impurities is flowed into as gas phase light component after condensation
In light component tank.
The column bottom temperature of the dehydration extracting tower is 130-135 DEG C, and tower top temperature is 70-80 DEG C；The bottom of tower temperature for the treatment of column
Degree is 135-140 DEG C, and tower top temperature is 100-104 DEG C；The de- light kettle bottom temperature is 98-102 DEG C, and kettle top temperature is 86-
90℃。
The characteristic of water is dissolved in insoluble in aldehyde using acid, after thick aldehyde is pumped into dehydration extracting tower, is dehydrated the bottom of tower of extracting tower
Temperature control is 130-135 DEG C, and tower top temperature control is 70-80 DEG C, and sour water becomes gas phase and runs up at this time, and aldehyde is liquid phase
It is scattered in bottom of tower downwards, since the tower body height of dehydration extracting tower increases, conversion zone is increased, accordingly increases the reflux of sour water
Amount, reduces the dosage of water so that gas-liquid phase separation is thorough, from the middle part feeding of dehydration extracting tower, is conducive to point of sour water and aldehyde
From being carried out at the same time to reach dehydration depickling, the places dehydration extracting tower 8-10m are equipped with filler, that is to say, that filler is installed in anti-
It answers section, filler to be changed to perforated plate corrugated filler by original float valve tray, further enhances the filterability in tower, so that sour
Water and aldehyde thoroughly detach.
Liquid branch device is installed at the top of dehydration extracting tower, increases reflux, regurgitant volume is increased to 100-200kg, is conducive to
The sour water taken off is passed back into again in dehydration extracting tower, and a small amount of sour water left in furfural is made to be further backing out.Sour water becomes
To be further recovered by condenser after gas phase in thick aldehyde original fluid container, reduces repeatedly addition and use a large amount of clear water, reduce
Waste, sour water circulating repetition of the present invention carry out dehydration depickling reaction, wherein no less than 3% aldehyde also recycles simultaneously, reduce aldehyde
Loss, reduces facility load, energy-saving.
Using the furfural finished product detection of furfural finished product and prior art production prepared by device of the present invention and technique
It is compared, testing result is shown in Table 1, the results show that the furfural finished product purity that the present invention is produced reaches 99.5%, smart aldehyde returns
Yield improves 3%-5% than of the same trade.
Table 1
| National standard | The produced furfural of the present invention | Existing method produces furfural | |
| Moisture % | 0.2 | 0.1 | 0.15 |
| Acidity mol/L | 0.016 | 0.01 | 0.014 |
| Furfural content % | 98.5 | 99.5 | 99 |
Claims (5)
1. a kind of refined furfural is dehydrated deacidifying device, it is characterised in that：Including being equipped with liquid level gauge（1）Thick aldehyde original fluid container（2）, slightly
Aldehyde original fluid container（2）Liquid outlet pumped by hair aldehyde（3）With high-order storage tank（4）Connection, high-order storage tank（4）Liquid outlet connection dehydration
Extracting tower（5）The inlet at middle part（5.1）, it is dehydrated extracting tower（5）Bottom and treating column（6）Connection, treating column（6）It installs at top
Condenser I（7）, condenser I（7）Liquid outlet connect finished product aldehyde tank（8）, condenser I（7）Slag notch connect raffinate kettle（9）,
Raffinate kettle（9）Liquid outlet connects thick aldehyde original fluid container（2）；It is dehydrated extracting tower（5）Install liquid distribution trough in top（10）, liquid distribution
Device（10）Install condenser II in top（11）, condenser II（11）Liquid outlet pass through gas-liquid separator（12）Connection layering tank
（13）And liquid distribution trough（10）, it is layered tank（13）Upper liquid outlet connection takes off light system, is layered tank（13）Bottom liquid goes out
Mouth passes through static tank（14）Connect thick aldehyde tank（15）, the de- light system is that top is connected with condenser III（16）De- light kettle
（17）, take off light kettle（17）Bottom connects thick aldehyde original fluid container（2）, condenser III（16）Liquid outlet connect light component tank（18）；Institute
The height for stating dehydration extracting tower is 11.3m, and the height of conversion zone is 10.01m, is dehydrated the inlet of extracting tower（5.1）Set on anti-
It answers at section 6-7m；It is dehydrated in extracting tower and 3 sections of fillers is set, every section of 3m, the filler is perforated plate corrugated filler, and parameter is：450Y/
∅698。
2. a kind of refined furfural according to claim 1 is dehydrated deacidifying device, it is characterised in that：The finished product aldehyde tank（8）
And gas-liquid separator（12）It is connected separately with vacuum tank, vacuum pump is installed at the top of vacuum tank, bottom is equipped with sewage draining exit.
3. a kind of refined furfural according to claim 1 is dehydrated deacidifying device, it is characterised in that：The dehydration extracting tower,
Treating column and the bottom for taking off light kettle are equipped with steam heater.
4. refining the technique of furfural using any refined furfural dehydration deacidifying device of claims 1 to 33, feature exists
In：The specific steps are：Thick aldehyde is pumped into high-order storage tank by hair aldehyde pump from thick aldehyde original fluid container, and the hair aldehyde in high-order storage tank enters de-
It is reacted in the middle part of water extracting tower, aqueous acid becomes vapour phase by liquid phase, runs up recycling, and aldehyde becomes liquid phase and runs down；
Aldehyde liquid is distributed to bottom of tower and flows into treating column, is further condensed back in treating column in income finished product aldehyde tank, and residue is discharged into raffinate kettle,
Residue is discharged raffinate kettle, and liquid is condensed back in the thick aldehyde original fluid container of income；Aqueous acid enters condenser into one after becoming gas phase
Step is condensed into liquid phase, and aqueous acid passes back into layering tank by gas-liquid separator, and after being layered in layering tank, sour water enters de-
Light system, aldehyde are recovered into thick aldehyde tank after static tank is static, and the sour water in de- light system detaches in taking off light kettle, aqueous acid
Thick aldehyde original fluid container is added by de- light bottom portion as liquid phase, organic impurities flows into light component as gas phase light component after condensation
In tank.
5. the technique according to claim 4 for being refined furfural using the refined furfural dehydration deacidifying device, feature are existed
In：The column bottom temperature of the dehydration extracting tower is 130-135 DEG C, and tower top temperature is 70-80 DEG C；The column bottom temperature for the treatment of column is
135-140 DEG C, tower top temperature is 100-104 DEG C；The de- light kettle bottom temperature is 98-102 DEG C, and kettle top temperature is 86-90 DEG C.
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| CN201510995139.9A CN105461669B (en) | 2015-12-28 | 2015-12-28 | A kind of refined furfural dehydration deacidifying device and process for refining |
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| CN105461669B true CN105461669B (en) | 2018-10-30 |
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| CN108929290A (en) * | 2018-08-12 | 2018-12-04 | 河南禾力能源股份有限公司 | A kind of furfural dehydration device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204051037U (en) * | 2014-08-19 | 2014-12-31 | 衡水中科信能源有限公司 | Furfural continuous rectification apparatus |
| CN204058311U (en) * | 2014-08-14 | 2014-12-31 | 河北中科智联节能科技股份公司 | The tower continuous treater of furfural production six |
| CN204428866U (en) * | 2014-12-04 | 2015-07-01 | 子洲县元嘉糠醛生产销售有限公司 | A kind of furfural extraction unit |
| CN204543613U (en) * | 2015-02-28 | 2015-08-12 | 衡水中科信能源有限公司 | Furfural batch fractionating process units |
-
2015
- 2015-12-28 CN CN201510995139.9A patent/CN105461669B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204058311U (en) * | 2014-08-14 | 2014-12-31 | 河北中科智联节能科技股份公司 | The tower continuous treater of furfural production six |
| CN204051037U (en) * | 2014-08-19 | 2014-12-31 | 衡水中科信能源有限公司 | Furfural continuous rectification apparatus |
| CN204428866U (en) * | 2014-12-04 | 2015-07-01 | 子洲县元嘉糠醛生产销售有限公司 | A kind of furfural extraction unit |
| CN204543613U (en) * | 2015-02-28 | 2015-08-12 | 衡水中科信能源有限公司 | Furfural batch fractionating process units |
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