CN105481803B - The technique and device of the semicontinuous refined furfural of continuous washing - Google Patents
The technique and device of the semicontinuous refined furfural of continuous washing Download PDFInfo
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- CN105481803B CN105481803B CN201610004666.3A CN201610004666A CN105481803B CN 105481803 B CN105481803 B CN 105481803B CN 201610004666 A CN201610004666 A CN 201610004666A CN 105481803 B CN105481803 B CN 105481803B
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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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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to the technique and device of a kind of semicontinuous refined furfural of continuous washing.Its step is：Dilute aldehyde hydrolyzate is obtained into aldehyde water mixed steam after primary distillation tower separates, is changed into liquid after the condensed device condensation of aldehyde water mixed steam, is layered into aldehyde tank is divided；Aldehyde after layering mutually enters water scrubber, and thick aldehyde storage tank is entered after the washing aldehyde metering after washing as refined materials；Thick aldehyde after washing starts warm tower into treating column, and through refined condenser, phase-splitter, aldehyde tank, head aldehyde liquid are put into thick aldehyde storage tank to tower top fraction after standing to the end successively；Warm tower closes head aldehyde tank valve after terminating, and water aldehyde is put into drain sump after phase-splitter；Subnatant is put into thick aldehyde storage tank after aldehyde water standing separation in drain sump, and dehydration aldehyde is stored in kettle；After dehydration terminates, dehydration aldehyde removes high component through treating column, by tower top successively through refined condenser, phase-splitter to smart aldehyde storage tank；Partially liq passes back into tower control product quality, is finally putting into smart aldehyde storage tank.The present invention can improve refined rate, improve product quality.
Description
Technical field
The present invention relates to furfural production method, the technique and device of specifically a kind of semicontinuous refined furfural of continuous washing.
Background technology
At present, during furfural production most of producers using plus alkali in and technique, then refined with an interval refining kettle
Into furfural product, there is a filled column on refining kettle.Thick aldehyde is disposably squeezed into refining kettle when refined, then is passed through steam heating
It is evaporated under reduced pressure, was both first steamed the moisture content of thick aldehyde and Light ends, then second step again steams smart aldehyde.This technique separation
Effect is poor, and the quantity that water aldehyde takes away furfural is more, and refined rate is low, and its average value is 81.3%；Thick aldehyde dehydration refines to enter at one pot
OK, increase when furfural is heated and inevitably cause allergic reaction；Because rectifying condition should not control, make its product quality inadequate
It is stable.
The content of the invention
Present invention seek to address that above mentioned problem existing for prior art, and refined rate can be improved, improve production by providing one kind
The technique and device of the semicontinuous refined furfural of continuous washing of quality.
The present invention solves the technical scheme that its technical problem uses：
A kind of technique of the semicontinuous refined furfural of continuous washing, is carried out in the steps below：
（1）Dilute aldehyde hydrolyzate is obtained into aldehyde water mixed steam after primary distillation tower separates, after the condensed device condensation of aldehyde water mixed steam
It is changed into liquid, is layered into aldehyde tank is divided；Water layer enters primary distillation tower recovery after de- light tank discharge Light ends after washing；
（2）Aldehyde after layering mutually enters water scrubber, and thick aldehyde storage tank is entered after the washing aldehyde metering after washing as refined materials；
（3）Thick aldehyde after washing starts warm tower into treating column, and tower top fraction is successively through refining condenser, phase-splitter to the end
Aldehyde tank, head aldehyde liquid are put into thick aldehyde storage tank after standing；
（4）Warm tower closes head aldehyde tank valve after terminating, and water aldehyde is put into drain sump after phase-splitter；The aldehyde water in drain sump
Subnatant is put into thick aldehyde storage tank after standing separation, and upper liquid is stored in kettle as tower water, dehydration aldehyde is washed；
（5）After dehydration terminates, dehydration aldehyde removes high component through treating column, by tower top successively through refined condenser, phase-splitter
To smart aldehyde storage tank；Partially liq passes back into tower control product quality, is finally putting into smart aldehyde storage tank.
A kind of device of the semicontinuous refined furfural of continuous washing, including primary distillation tower, water scrubber, treating column, in addition to divide aldehyde
Tank, take off light tank, phase-splitter；
The aldehyde water mixing vapor outlet connection condenser of fore-running column overhead, the liquid-phase outlet connection of condenser divide aldehyde tank, divide aldehyde
The aldehyde of tank mutually exports connection water scrubber, and the washing aldehyde outlet of water scrubber connects thick aldehyde storage tank, the thick aldehyde of thick aldehyde storage tank through measuring tank
Outlet connects treating column through spinner flowmeter, refines the refined condenser of fraction outlet connection of column overhead, refines the liquid of condenser
Mutually outlet connection phase-splitter, the head aldehyde outlet port connector aldehyde tank of phase-splitter, the thick aldehyde outlet connection drain sump of phase-splitter, phase-splitter
The outlet of smart aldehyde connect smart aldehyde storage tank, head aldehyde tank, the thick aldehyde refluxing opening of drain sump connect thick aldehyde storage tank；Divide the water layer backflow of aldehyde tank
Mouth connection primary distillation tower；The water layer outlet connection of water scrubber takes off light tank, takes off the refluxing opening connection primary distillation tower of light tank.
Further, in addition to vavuum pump the vacuum tank being connected, vacuum tank are connected with drain sump.
Using the present invention of above-mentioned technical proposal, compared with prior art, its advantage is：
（1）Will interval is refined is changed to that continuous washing is semicontinuous refined, aqueous chaff aldehyde after washing is 5.5% or so, gently
Component reduces 50%, and acidity is 0.02 equivalents per liter or so, improves thick aldehyde purity, can shorten when refined the head section time 1~
1.2 hours, its refined rate average value was 91.7%, and reduces the water in subtractive process, electricity, vapour consumption, and smart aldehyde per ton is reduced
0.2 ton of steam consumption.
（2）Because WATER-WASHING METHOD completely dispenses with alkali, so as to eliminate because alkali neutralizes the sodium acetate made containing surplus in thick aldehyde,
Into treating column, cause the decomposition of furfural in subtractive process, the problem of polymerization, refined rate can improve；
（3）Only larger neutralizing tank is replaced with the tower of a very little, not only reduce equipment investment, and also save because
The consumed electric power of stirring.
（4）Improve operation condition, eliminate interval neutralize be not easy sealing and caused by environmental pollution.
（5）Continuous washing, it is simple to operate easily to grasp, operator's labor intensity can be mitigated.
Brief description of the drawings
Fig. 1 is the apparatus structure and process flow diagram of the embodiment of the present invention；
In figure：1- stoste head tanks；2- primary distillation towers；3- condensers；4- divides aldehyde tank；5- water scrubbers；6- takes off light tank；7- is measured
Tank；The thick aldehyde storage tanks of 8-；9- treating columns；10- spinner flowmeters；11- refines condenser；12- phase-splitters；13- head aldehyde tanks；14- takes off
Water pot；15- essence aldehyde storage tanks；16- vacuum tanks.
Embodiment
The present invention is further elaborated with reference to embodiments, but embodiment does not form any restrictions to the present invention.
Referring to Fig. 1, a kind of device of the semicontinuous refined furfural of continuous washing, by stoste head tank 1, primary distillation tower 2, condenser
3rd, divide aldehyde tank 4, water scrubber 5, take off light tank 6, measuring tank 7, thick aldehyde storage tank 8, treating column 9, spinner flowmeter 10, refined condenser
11st, phase-splitter 12, head aldehyde tank 13, drain sump 14, smart aldehyde storage tank 15, vacuum tank 16 are connected and composed by pipeline, are specifically：
The aldehyde water mixing vapor outlet connection condenser 3 of the tower top of primary distillation tower 2, the liquid-phase outlet connection of condenser 3 divide aldehyde tank 4,
The aldehyde of aldehyde tank 4 is divided mutually to export connection water scrubber 5, the washing aldehyde outlet of water scrubber 5 connects thick aldehyde storage tank 8, thick aldehyde storage through measuring tank 7
The thick aldehyde outlet of tank 8 connects treating column 9 through spinner flowmeter 11, and the fraction outlet connection of the tower top for the treatment of column 9 refines condenser 11,
The liquid-phase outlet connection phase-splitter 12 of refined condenser 11, the head aldehyde outlet port connector aldehyde tank 13 of phase-splitter 12, phase-splitter 12
Thick aldehyde outlet connection drain sump 14, drain sump 14 connect vacuum tank 16, and the smart aldehyde outlet of phase-splitter 12 connects smart aldehyde storage tank 15, head
Aldehyde tank 13, the thick aldehyde refluxing opening of drain sump 14 connect thick aldehyde storage tank 8；Divide the water layer refluxing opening connection primary distillation tower 2 of aldehyde tank 4；Washing
The water layer outlet connection of tower 5 takes off light tank 6, takes off the refluxing opening connection primary distillation tower 2 of light tank 6.
The technique of the above-mentioned semicontinuous refined furfural of continuous washing, is carried out in the steps below：
（1）Dilute aldehyde hydrolyzate from stoste head tank 1, enter primary distillation tower 2, the tower reactor of primary distillation tower 2 is heated using aldehyde vapour, directly
Connect steam to be discharged by tower reactor as supplement waste water, the condensed device 3 of the aldehyde water mixed steam that tower top is drawn is changed into liquid after condensing, and enters
Divide aldehyde tank 4；Water layer enters primary distillation tower 2 and reclaimed after de- light tank 6 discharges Light ends after washing.
（2）Water layer after layering passes back into primary distillation tower 2, and aldehyde mutually enters water scrubber 5, and the washing aldehyde after washing enters measuring tank 7, meter
Enter thick aldehyde storage tank 8 after amount as refined materials, water layer enters primary distillation tower 2 and reclaimed after de- light tank 6 discharges Light ends after washing.
（3）Thick aldehyde after washing, through spinner flowmeter 10, start warm tower into treating column 9, tower top fraction is through refined condensation
Device 11 crosses the aldehyde tank 13 to the end of phase-splitter 12；Head aldehyde liquid is put into thick aldehyde storage tank 8 after standing.
（4）Warm tower closes the valve of head aldehyde tank 13 after terminating, water aldehyde is put into drain sump 14 after phase-splitter 12；In drain sump
Subnatant is put into thick aldehyde storage tank 8 after aldehyde water standing separation in 14, and upper liquid is stored in kettle as tower water, dehydration aldehyde is washed；
（5）After dehydration terminates, dehydration aldehyde removes high component through treating column 9, by tower top successively through refined condenser 11, split-phase
Device 12 arrives smart aldehyde storage tank 15；Partially liq passes back into tower control product quality, is finally putting into smart aldehyde storage tank 15.
Preferably feasible embodiment of the invention is the foregoing is only, not thereby limits to the interest field of the present invention,
All equivalence changes made with present specification, it is both contained within the interest field of the present invention.
Claims (3)
1. a kind of technique of the semicontinuous refined furfural of continuous washing, it is characterised in that carry out in the steps below：
（1）Dilute aldehyde hydrolyzate is obtained into aldehyde water mixed steam after primary distillation tower separates, is changed into after the condensed device condensation of aldehyde water mixed steam
Liquid, it is layered into aldehyde tank is divided；Water layer enters primary distillation tower recovery after de- light tank discharge Light ends after washing；
（2）Aldehyde after layering mutually enters water scrubber, and thick aldehyde storage tank is entered after the washing aldehyde metering after washing as refined materials；
（3）Thick aldehyde after washing starts warm tower into treating column, and tower top fraction is successively through refining condenser, phase-splitter aldehyde to the end
Tank, head aldehyde liquid are put into thick aldehyde storage tank after standing；
（4）Warm tower closes head aldehyde tank valve after terminating, and water aldehyde is put into drain sump after phase-splitter；Aldehyde water is stood in drain sump
Subnatant is put into thick aldehyde storage tank after separation, and upper liquid is used as and washes tower water；Dehydration aldehyde is stored in treating column tower reactor；
（5）After dehydration terminates, dehydration aldehyde removes high component through treating column, by tower top successively through refined condenser, phase-splitter to essence
Aldehyde storage tank；Partially liq passes back into tower control product quality, is finally putting into smart aldehyde storage tank.
2. a kind of device of semicontinuous refined furfural of continuous washing for described in claim 1, including primary distillation tower, water scrubber,
Treating column, it is characterised in that：
Also include dividing aldehyde tank, take off light tank, phase-splitter；
The aldehyde water mixing vapor outlet connection condenser of fore-running column overhead, the liquid-phase outlet connection of condenser divide aldehyde tank, divide aldehyde tank
Aldehyde mutually exports connection water scrubber, and the washing aldehyde outlet of water scrubber connects thick aldehyde storage tank, the thick aldehyde outlet of thick aldehyde storage tank through measuring tank
Treating column is connected through spinner flowmeter, refines the refined condenser of fraction outlet connection of column overhead, the liquid phase of refined condenser goes out
Mouth connection phase-splitter, the head aldehyde outlet port connector aldehyde tank of phase-splitter, the thick aldehyde outlet connection drain sump of phase-splitter, the essence of phase-splitter
Aldehyde outlet connects smart aldehyde storage tank, and head aldehyde tank, the thick aldehyde refluxing opening of drain sump connect thick aldehyde storage tank；The water layer refluxing opening of aldehyde tank is divided to connect
Connect primary distillation tower；The water layer outlet connection of water scrubber takes off light tank, takes off the refluxing opening connection primary distillation tower of light tank.
3. the device of the semicontinuous refined furfural of continuous washing according to claim 2, it is characterised in that also include and vacuum
The vacuum tank of pump connection, vacuum tank are connected with drain sump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610004666.3A CN105481803B (en) | 2016-01-07 | 2016-01-07 | The technique and device of the semicontinuous refined furfural of continuous washing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610004666.3A CN105481803B (en) | 2016-01-07 | 2016-01-07 | The technique and device of the semicontinuous refined furfural of continuous washing |
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| Publication Number | Publication Date |
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| CN105481803A CN105481803A (en) | 2016-04-13 |
| CN105481803B true CN105481803B (en) | 2018-02-16 |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086180B (en) * | 2010-11-23 | 2013-01-09 | 山东省阳信金缘纺化有限公司 | Process for improving furfural yield and aldehyde-water separation device utilized thereby |
| CN104130224B (en) * | 2014-08-14 | 2016-04-06 | 河北中科智联节能科技股份公司 | The tower continuous treater of furfural production six and furfural treatment technique thereof |
| CN104645656A (en) * | 2015-02-28 | 2015-05-27 | 衡水中科信能源有限公司 | Furfural batch distillation production device and process |
| CN205295196U (en) * | 2016-01-07 | 2016-06-08 | 唐山宏文有机肥料有限公司 | Wash device of semicontinuous refined furfural in succession |
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Effective date of registration: 20220210 Address after: 063700 Gu Ma Zhen Xing Long Zhuang Cun Xi, luanzhou City, Tangshan City, Hebei Province Patentee after: Luanzhou luanxing Biotechnology Co.,Ltd. Address before: 063100 north of Jinghua Road, Guye District, Tangshan City, Hebei Province Patentee before: TANGSHAN HONGWEN ORGANIC FERTILIZER Co.,Ltd. |
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