CN105461669A - Dehydration and deacidification device for refining furfural and refining process - Google Patents
Dehydration and deacidification device for refining furfural and refining process Download PDFInfo
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- CN105461669A CN105461669A CN201510995139.9A CN201510995139A CN105461669A CN 105461669 A CN105461669 A CN 105461669A CN 201510995139 A CN201510995139 A CN 201510995139A CN 105461669 A CN105461669 A CN 105461669A
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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 the technical field of a production process of a chemical product of furfural. In order to solve the problems of wastes, increase of equipment burden and the like caused by the reason that dehydration and deacidification are not thorough during furfural production and aldehyde is taken away during dehydration and deacidification, the invention provides a dehydration and deacidification device for refining furfural and a refining process. According to the refining process, crude furfural is subjected to reaction in a dehydration and deacidification tower, acid water changes from a liquid phase to a vapor phase and moves upwards for recovery, aldehyde is changed into a liquid phase and flows downwards into a refining tower, finished product aldehyde is recovered through condensation in the refining tower, and resides are discharged out; and the acid water enters a condenser and changes into a liquid phase, part of the acid water flows back into the dehydration and deacidification tower, part of the acid water flows into a layering tank for layering, the aldehyde is recovered into a crude aldehyde tank after being motionless, the acid water is added into a crude aldehyde stock solution tank from the bottom of a light removing kettle, and organic impurities flow into a light component tank after condensation. Acid of crude aldehyde is recovered completely, the recovery rate of refined aldehyde is improved by 3-5% compared with that of the same industry, the purity of furfural is improved to more than 99.5%, and the quality of the refined aldehyde is stabilized to a premium grade, so that the demands of high-end users on the market can be met.
Description
Technical field
The invention belongs to chemical preparations furfural production technology technical field, be specifically related to a kind of refining furfural dehydration deacidifying device and process for refining.
Background technology
Two kinds of dehydration acid stripping methods of the current furfural production of China are: use soda ash neutralisation: sulfuric acid is neutralized neutrality, then dewater by distillation method; Wash method with water: utilize the water-soluble characteristic being insoluble to aldehyde of sulfuric acid, with the acid in a large amount of clear water dilution furfural, reach the effect of depickling.
Above two kinds of acid stripping methods all have a significant impact the furfural rate of recovery, and first method makes furfuryl resin in treating process, and form aldehyde mud, the rate of recovery is low; Second method uses a large amount of clear water, will take away the aldehyde being no less than 3%, cannot reclaim while dehydration depickling, and the water of depickling simultaneously causes loss and the waste of heat through waste water evaporator evaporation, both added facility load, and be also unfavorable for saving energy and reduce the cost.
Soda ash neutralisation, the organic side reaction causing furfural itself under condition or occur with other materials in solution.Cause the generation of not clear material.Thus cause the loss of furfural.Affect the rate of recovery of furfural and the purity of furfural.
And WATER-WASHING METHOD utilizes the water-soluble characteristic being insoluble to aldehyde of acid, dilute the acid in thick aldehyde (water of 10%, the aldehyde of 90%) with a large amount of softening clear water, go out water, the acid of thick aldehyde by water-band, reach the effect of depickling.This kind of method wastes a large amount of softening clear water, and 1 ton of thick aldehyde need use 0.3-0.5 ton water.Lose thick aldehyde, in clear water, take away the aldehyde being not less than 3%.Process aldehyde water is by steam heating, needs to waste heat energy.
Summary of the invention
The present invention is not thorough in order to solve in existing furfural production depickling of dewatering, and takes away aldehyde in dehydration deacidification simultaneously, causes causing waste, increasing the problems such as facility load, provides a kind of refining furfural dehydration deacidifying device and process for refining.
The present invention is realized by following technical scheme: a kind of refining furfural dehydration deacidifying device, comprise the thick aldehyde original fluid container being provided with liquidometer, the liquid outlet of thick aldehyde original fluid container is connected with high-order storage tank by hair aldehyde pump, the liquid outlet of high-order storage tank connects the fluid inlet in the middle part of dehydration extracting tower, be connected with treating tower bottom dehydration extracting tower, condenser I is installed at treating tower top, and the liquid outlet of condenser I connects finished product aldehyde tank, the slag notch of condenser I connects raffinate still, and raffinate liquid from reactor mouth connects thick aldehyde original fluid container; Liquid distributor is installed at dehydration extracting tower top, condenser II is installed on liquid distributor top, the liquid outlet of condenser II connects layering tank and liquid distributor by gas-liquid separator, the outlet of layering tank upper liquid connects de-light system, layering pot bottom liquid exit connects thick aldehyde tank by static tank, described de-light system is the de-light still that top is connected with condenser III, connects thick aldehyde original fluid container bottom de-light still, and the liquid outlet of condenser III connects light constituent tank.
The height of described dehydration extracting tower is 11.3m, and the height of conversion zone is 10.01m, and the fluid inlet of dehydration extracting tower is located at conversion zone 6-7m place; Arrange 3 sections of fillers, every section of 3m in dehydration extracting tower, described filler is perforated plate corrugated filler, and parameter is: 450Y/ 698.
Described finished product aldehyde tank and gas-liquid separator are connected to vacuum tank, and vacuum pump is installed at vacuum tank top, and bottom is provided with sewage draining exit.The bottom of described dehydration extracting tower, treating tower and de-light still is provided with steam heater.
Described refining furfural dehydration deacidifying device is utilized to refine the technique of furfural, concrete steps are: thick aldehyde pumps into high-order storage tank by hair aldehyde pump from thick aldehyde original fluid container, the middle part that hair aldehyde in high-order storage tank enters dehydration extracting tower is reacted, aqueous acid becomes vapour phase by liquid phase, upwards run recovery, aldehyde becomes liquid phase and runs downwards; Aldehyde liquid is distributed to tower bottom flow and enters treating tower, and in treating tower, further condensation is recovered in finished product aldehyde tank, and residue enters raffinate still, and residue is discharged by raffinate still, and condenses is recovered in thick aldehyde original fluid container; Aqueous acid enters condenser after becoming gas phase and is condensed into liquid phase further, aqueous acid passes through gas-liquid separator, pass back into layering tank, in layering tank after layering, sour water enters de-light system, and aldehyde is recovered into thick aldehyde tank after static tank is static, and the sour water in de-light system is separated in de-light still, aqueous acid adds thick aldehyde original fluid container as liquid phase by taking off bottom light still, and organic impurity flows in light constituent tank as gas phase light constituent after condensation.
The column bottom temperature of described 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 tower is 135-140 DEG C, and tower top temperature is 100-104 DEG C; At the bottom of described de-light still still, temperature is 98-102 DEG C, and still top temperature is 86-90 DEG C.The light constituent that de-light system removes is the organic impuritys such as a small amount of formaldehyde, acetone; Vacuum tank, for be vacuumized by surge tank, makes whole system be in negative pressure state.
Acid is utilized to be insoluble to aldehyde and water-soluble characteristic, after thick aldehyde being pumped into dehydration extracting tower, the column bottom temperature of dehydration extracting tower controls as 130-135 DEG C, tower top temperature controls as 70-80 DEG C, now sour water becomes gas phase and upwards runs, and aldehyde is liquid phase is scattered in downwards at the bottom of tower, because the tower body height of the extracting tower that dewaters increases, add conversion zone, the corresponding quantity of reflux adding sour water, decrease the consumption of water, liquid phase is made to be separated thoroughly, from the middle part material loading of dehydration extracting tower, be beneficial to being separated of sour water and aldehyde, thus reach dehydration depickling carry out simultaneously, dehydration extracting tower 8-10m place is provided with filler, that is filler is installed in conversion zone, filler changes perforated plate corrugated filler into by original valve tray, further enhance the filterableness in tower, thus sour water is separated thoroughly with aldehyde.
Liquid branch device is installed at the top of dehydration extracting tower, and add backflow, quantity of reflux brings up to 100-200kg, is beneficial to the sour water taken off and passes back into again in dehydration extracting tower, a small amount of sour water left in furfural is deviate from further.Be recovered into further in the static tank of layering by condenser after sour water becomes gas phase, decrease waste, sour water of the present invention is cycled to repeat and carries out dehydration depickling reaction, the aldehyde being wherein no less than 3% also reclaims simultaneously, decrease the loss of aldehyde, reduce facility load, energy-saving and cost-reducing.
The present invention utilizes acid to be insoluble to aldehyde and water-soluble characteristic, dehydration depickling is synchronously carried out; Utilize perforated plate corrugated filler, strengthen filterableness; The tower body height of dehydration extracting tower increases, and adds conversion zone, adds the quantity of reflux of sour water accordingly, from the middle part material loading of dehydration extracting tower, is beneficial to and makes sour water become vapour phase from liquid phase, upwards run recovery; And aldehyde still runs downwards for liquid phase, be convenient to sour water to be separated with aldehyde, thus reach dehydration depickling carry out simultaneously.Liquid branch device is installed at the top of dehydration extracting tower, adds backflow, is beneficial to the sour water taken off and passes back into again in dehydration extracting tower, a small amount of sour water left in furfural is deviate from further.
The present invention is run by test of many times, and after testing, the acid of thick aldehyde has been carried out reclaiming completely, the rate of recovery of essence aldehyde improves 3%-5% than of the same trade, the purity of furfural brings up to more than 99.5%, and the steady quality of smart aldehyde, to top grade product, can meet the demand of market high-end user.
Accompanying drawing explanation
Fig. 1 is refining furfural dehydration deacidifying device structural representation of the present invention, and Fig. 2 is process flow sheet of the present invention.
In figure: 1-liquidometer; The thick aldehyde original fluid container of 2-; 3-hair aldehyde pump; The high-order storage tank of 4-; 5-dewaters extracting tower; 5.1-fluid inlet; 6-treating tower; 7-condenser I; 8-finished product aldehyde tank; 9-raffinate still; 10-liquid distributor; 11-condenser II; 12-gas-liquid separator; 13-layering tank; The static tank of 14-; The thick aldehyde tank of 15-; 16-condenser III; 17-takes off light still; 18-light constituent tank.
Embodiment
A kind of refining furfural dehydration deacidifying device, comprise the thick aldehyde original fluid container 2 being provided with liquidometer 1, the liquid outlet of thick aldehyde original fluid container 2 is connected with high-order storage tank 4 by hair aldehyde pump 3, the liquid outlet of high-order storage tank 4 connects the fluid inlet 5.1 in the middle part of dehydration extracting tower 5, be connected with treating tower 6 bottom dehydration extracting tower 5, condenser I7 is installed at treating tower 6 top, and the liquid outlet of condenser I7 connects finished product aldehyde tank 8, the slag notch of condenser I7 connects raffinate still 9, and raffinate still 9 liquid outlet connects thick aldehyde original fluid container 2; Liquid distributor 10 is installed at dehydration extracting tower 5 top, condenser II11 is installed on liquid distributor 10 top, the liquid outlet of condenser II11 connects layering tank 13 and liquid distributor 10 by gas-liquid separator 12, the outlet of layering tank 13 upper liquid connects de-light system, layering tank 13 bottom liquid outlet connects thick aldehyde tank 15 by static tank 14, described de-light system is the de-light still 17 that top is connected with condenser III16, connect thick aldehyde original fluid container 2 bottom de-light still 17, the liquid outlet of condenser III16 connects light constituent tank 18.
The height of described dehydration extracting tower is 11.3m, and the height of conversion zone is 10.01m, and the fluid inlet 5.1 of dehydration extracting tower is located at conversion zone 6-7m place; Arrange 3 sections of fillers, every section of 3m in dehydration extracting tower, described filler is perforated plate corrugated filler, and parameter is: 450Y/ 698.Described finished product aldehyde tank 8 and gas-liquid separator 12 are connected to vacuum tank, and vacuum pump is installed at vacuum tank top, and bottom is provided with sewage draining exit.The bottom of described dehydration extracting tower, treating tower and de-light still is provided with steam heater.
Refining furfural dehydration deacidifying device described in utilization refines the technique of furfural, concrete steps are: thick aldehyde pumps into high-order storage tank by hair aldehyde pump from thick aldehyde original fluid container, the middle part that hair aldehyde in high-order storage tank enters dehydration extracting tower is reacted, aqueous acid becomes vapour phase by liquid phase, upwards run recovery, aldehyde becomes liquid phase and runs downwards; Aldehyde liquid is distributed to tower bottom flow and enters treating tower, and in treating tower, further condensation is recovered in finished product aldehyde tank, and residue enters raffinate still, and residue is discharged by raffinate still, and condenses is recovered in thick aldehyde original fluid container; Aqueous acid enters condenser after becoming gas phase and is condensed into liquid phase further, aqueous acid passes through gas-liquid separator, partial reflux enter to dewater extracting tower continue reaction, part flows into layering tank, and in layering tank after layering, sour water enters de-light system, aldehyde is recovered into thick aldehyde tank after static tank is static, sour water in de-light system is separated in de-light still, and aqueous acid adds thick aldehyde original fluid container as liquid phase by taking off bottom light still, and organic impurity flows in light constituent tank as gas phase light constituent after condensation.
The column bottom temperature of described 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 tower is 135-140 DEG C, and tower top temperature is 100-104 DEG C; At the bottom of described de-light still still, temperature is 98-102 DEG C, and still top temperature is 86-90 DEG C.
Acid is utilized to be insoluble to aldehyde and water-soluble characteristic, after thick aldehyde being pumped into dehydration extracting tower, the column bottom temperature of dehydration extracting tower controls as 130-135 DEG C, tower top temperature controls as 70-80 DEG C, now sour water becomes gas phase and upwards runs, and aldehyde is liquid phase is scattered in downwards at the bottom of tower, because the tower body height of the extracting tower that dewaters increases, add conversion zone, the corresponding quantity of reflux adding sour water, decrease the consumption of water, liquid phase is made to be separated thoroughly, from the middle part material loading of dehydration extracting tower, be beneficial to being separated of sour water and aldehyde, thus reach dehydration depickling carry out simultaneously, dehydration extracting tower 8-10m place is provided with filler, that is filler is installed in conversion zone, filler changes perforated plate corrugated filler into by original valve tray, further enhance the filterableness in tower, thus sour water is separated thoroughly with aldehyde.
Liquid branch device is installed at the top of dehydration extracting tower, and add backflow, quantity of reflux brings up to 100-200kg, is beneficial to the sour water taken off and passes back into again in dehydration extracting tower, a small amount of sour water left in furfural is deviate from further.Be recovered in thick aldehyde original fluid container further by condenser after sour water becomes gas phase, decrease repeatedly to add and use a large amount of clear water, decrease waste, sour water of the present invention is cycled to repeat and carries out dehydration depickling reaction, the aldehyde being wherein no less than 3% also reclaims simultaneously, decrease the loss of aldehyde, reduce facility load, energy-saving and cost-reducing.
The furfural finished product detection of the furfural finished product prepared by device of the present invention and technique and existing explained hereafter is adopted to compare, detected result is in table 1, result shows, and the furfural finished product purity that the present invention produces reaches 99.5%, and the rate of recovery of smart aldehyde improves 3%-5% than of the same trade.
Table 1
| National standard | The present invention produces furfural | Existing method produces furfural | |
| Moisture content % | 0.2 | 0.1 | 0.15 |
| Acidity mol/L | 0.016 | 0.01 | 0.014 |
| Furfural content % | 98.5 | 99.5 | 99 |
Claims (6)
1. a refining furfural dehydration deacidifying device, it is characterized in that: comprise the thick aldehyde original fluid container (2) being provided with liquidometer (1), the liquid outlet of thick aldehyde original fluid container (2) is connected with high-order storage tank (4) by hair aldehyde pump (3), the liquid outlet of high-order storage tank (4) connects the fluid inlet (5.1) at dehydration extracting tower (5) middle part, dehydration extracting tower (5) bottom is connected with treating tower (6), condenser I(7 is installed at treating tower (6) top), condenser I(7) liquid outlet connect finished product aldehyde tank (8), condenser I(7) slag notch connect raffinate still (9), raffinate still (9) liquid outlet connects thick aldehyde original fluid container (2), liquid distributor (10) is installed at dehydration extracting tower (5) top, condenser II(11 is installed on liquid distributor (10) top), condenser II(11) liquid outlet connect layering tank (13) and liquid distributor (10) by gas-liquid separator (12), the outlet of layering tank (13) upper liquid connects de-light system, layering tank (13) bottom liquid outlet connects thick aldehyde tank (15) by static tank (14), described de-light system is that top is connected with condenser III(16) de-light still (17), de-light still (17) bottom connects thick aldehyde original fluid container (2), condenser III(16) liquid outlet connect light constituent tank (18).
2. one according to claim 1 refines furfural dehydration deacidifying device, and it is characterized in that: the height of described dehydration extracting tower is 11.3m, the height of conversion zone is 10.01m, and the fluid inlet (5.1) of dehydration extracting tower is located at conversion zone 6-7m place; Arrange 3 sections of fillers, every section of 3m in dehydration extracting tower, described filler is perforated plate corrugated filler, and parameter is: 450Y/ 698.
3. one according to claim 1 refines furfural dehydration deacidifying device, it is characterized in that: described finished product aldehyde tank (8) and gas-liquid separator (12) are connected to vacuum tank, and vacuum pump is installed at vacuum tank top, and bottom is provided with sewage draining exit.
4. one according to claim 1 refines furfural dehydration deacidifying device, it is characterized in that: the bottom of described dehydration extracting tower, treating tower and de-light still is provided with steam heater.
5. utilize the refining furfural dehydration deacidifying device described in claim 1-4 to refine the technique of furfural, it is characterized in that: concrete steps are: thick aldehyde pumps into high-order storage tank by hair aldehyde pump from thick aldehyde original fluid container, the middle part that hair aldehyde in high-order storage tank enters dehydration extracting tower is reacted, aqueous acid becomes vapour phase by liquid phase, upwards run recovery, aldehyde becomes liquid phase and runs downwards; Aldehyde liquid is distributed to tower bottom flow and enters treating tower, and in treating tower, further condensation is recovered in finished product aldehyde tank, and residue enters raffinate still, and residue is discharged by raffinate still, and condenses is recovered in thick aldehyde original fluid container; Aqueous acid enters condenser after becoming gas phase and is condensed into liquid phase further, aqueous acid passes through gas-liquid separator, pass back into layering tank, in layering tank after layering, sour water enters de-light system, and aldehyde is recovered into thick aldehyde tank after static tank is static, and the sour water in de-light system is separated in de-light still, aqueous acid adds thick aldehyde original fluid container as liquid phase by taking off bottom light still, and organic impurity flows in light constituent tank as gas phase light constituent after condensation.
6. the technique utilizing described refining furfural dehydration deacidifying device to refine furfural according to claim 5, is characterized in that: the column bottom temperature of described 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 tower is 135-140 DEG C, and tower top temperature is 100-104 DEG C; At the bottom of described de-light still still, temperature is 98-102 DEG C, and still top temperature is 86-90 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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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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| 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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| CN105461669A true CN105461669A (en) | 2016-04-06 |
| CN105461669B CN105461669B (en) | 2018-10-30 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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2015
- 2015-12-28 CN CN201510995139.9A patent/CN105461669B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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