CN104130224B - The tower continuous treater of furfural production six and furfural treatment technique thereof - Google Patents
The tower continuous treater of furfural production six and furfural treatment technique thereof Download PDFInfo
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- CN104130224B CN104130224B CN201410399151.9A CN201410399151A CN104130224B CN 104130224 B CN104130224 B CN 104130224B CN 201410399151 A CN201410399151 A CN 201410399151A CN 104130224 B CN104130224 B CN 104130224B
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- aldehyde
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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
Abstract
The tower continuous treater of furfural production six and furfural treatment technique thereof, primarily of primary tower, dehydration tower and treating tower composition, increase de-with light packsly to put, water washing device and aldehyde mud retrieving arrangement, de-with light packs putting comprises lightness-removing column, water cooler and lightness-removing column overhead condenser; Water washing device comprises point aldehyde tank and a water wash column; Aldehyde mud retrieving arrangement comprises water aldehyde tank, recycle-water aldehyde tank and recovery tower.The present invention with light packsly to be put except the Light ends anhydrated in aldehyde decreases the concentration of the Light ends in primary tower by de-, improves primary tower efficiency and refining rate; Utilize water washing device to replace adding alkali neutralization, remove the organic acid in thick aldehyde, improve refining rate 4%, add economic benefit, primary tower waste water aldehyde contenting amount can be reduced simultaneously, reduce environmental pollution; Regularly reclaimed the furfural in aldehyde liquid by aldehyde mud retrieving arrangement, solve the loss that existing raffinate takes the bad recovery of furfural out of, in the foreshot of generation of simultaneously dewatering, furfural is reclaimed, and reduces in Furfural Treating Process and loses, improve furfural yield 5-6%.
Description
Technical field
The present invention relates to furfural production technical field, be specifically related to the tower continuous treater of a kind of furfural production six and furfural treatment technique thereof.
Background technology
Furfural production master mainly comprises two processes:
1, be hydrolyzed, the pentosan in plant is hydrolyzed to pentose through adding temperature under the effect of H+, and pentose is through heating under the effect of H+, and furfural is produced in dehydration further.
2, refining, refine being hydrolyzed the rare furfural hydrolysis liquid fractionation by distillation obtained, in removing hydrolyzed solution, institute is with a large amount of water, and a small amount of acetic acid, methyl alcohol, acetone, the contour lower-boiling impurity of first class furfural of generation when being hydrolyzed, and obtains qualified finished product furfural.
The rapider ultimate production of China's furfurol industry development accounted for more than 70% of the world in recent years, yearly capacity reaches 40-50 ten thousand tons, Xian Ge factory throughput is all expanding gradually, the factory that annual output scale is more than 5000 tons is a lot, the purchasing price of corn cob improves constantly, the height of furfural yield directly affects furfural production cost, improve yield in order to make rational use of resources and reduce consumption raising quality, each factory updates technique, in succession different process is used especially in the rectification flow of thick aldehyde, rectification flow changes three tower continuous rectifications into by most junior one tower one still technical process, three-tower type continuous refining process flow process, i.e. primary tower, dehydration tower, treating tower.
In current China furfural production, FF adopts three tower continuous treatings or interval process for refining mostly, but in treating process, Light ends is not separated participates in refining whole process, centre also will add rice bran water aldehyde liquid and take away a large amount of furfural foreshot and do not reclaim and be let go, furfural loss is larger, the refining rate of impact, furfural is lost in 6 ~ 7% in treating process.
Summary of the invention
The invention provides the tower continuous treater of a kind of furfural production six and furfural treatment technique thereof, the furfural existed to solve prior art loses the problem of refining rate than considerable influence.
The tower continuous treater of furfural production six of the present invention forms primarily of primary tower, dehydration tower and treating tower, solve technical scheme that its technical problem adopts be increase de-with light packsly to put, water washing device and aldehyde mud retrieving arrangement, de-with light packs putting comprises lightness-removing column, water cooler and lightness-removing column overhead condenser, the outlet of lightness-removing column tower reactor is connected with primary tower by water cooler, and lightness-removing column tower top is connected with lightness-removing column overhead condenser; Water washing device comprises point aldehyde tank and a water wash column, aldehyde tank top is divided to be connected with primary tower overhead condenser, aldehyde pot bottom is divided to be connected with the import of water wash column tower top, divide in the middle part of aldehyde tank and be connected with lightness-removing column opening for feed, water wash column tower top outlet is also connected with lightness-removing column opening for feed, water wash column outlet at bottom is connected with dehydration tower import, connects a back with water inlet line bottom water wash column; Aldehyde mud retrieving arrangement comprises water aldehyde tank, recycle-water aldehyde tank and recovery tower, water aldehyde tank top is connected with dehydration column overhead condenser, water aldehyde pot bottom is connected with lightness-removing column opening for feed with recycle-water aldehyde tank respectively, and recycle-water aldehyde pot bottom is connected with recovery tower top inlet together with bottom treating tower.
Above-mentioned primary tower, dehydration tower and treating tower all adopt valve tray column; Lightness-removing column, water wash column and recovery tower are sieve-tray tower.
The furfural treatment technique of the tower continuous treater of above-mentioned furfural production six, by de-with light packs putting, the light constituents such as methanol acetone are separated from water aldehyde, remove the organic acid in thick aldehyde by water washing device, regularly reclaimed the furfural in aldehyde liquid by aldehyde mud retrieving arrangement, concrete technology step is as follows:
(1) rare aldehyde hydrolyzed solution enters primary tower by original fluid container, and discharge containing high boiling material waste water at the bottom of tower, overhead vapours is condensate in layering in point aldehyde tank through primary tower overhead condenser;
(2) dividing the aqueous phase of layering in aldehyde tank to enter lightness-removing column, to enter lightness-removing column together with the aqueous phase of water wash column tower top and the water aldehyde at dehydration tower top de-light, aqueous phase at the bottom of lightness-removing column tower returns primary tower and refluxes after water cooler, extraction Light ends after the condensation of lightness-removing column overhead vapours, part overhead condensation liquid is back in lightness-removing column simultaneously;
(3) divide the aldehyde of aldehyde pot bottom to enter water wash column by water wash column top, intake bottom water wash column, aldehyde water is than being 1:1, and water wash column tower top aqueous phase removes lightness-removing column, and aldehyde at the bottom of water wash column tower send dehydration tower to dewater mutually;
(4) dehydration column overhead deviates from light fraction, dehydration aldehyde is discharged by dehydration tower tower reactor, dehydration aldehyde send treating tower to refine, light fraction enters water aldehyde tank through dehydration column overhead condenser condenses, after material layering in water aldehyde tank, it is de-light that upper materials enters lightness-removing column, and lower floor's material removes the furfural in recovery tower in recycle-water aldehyde through recycle-water aldehyde tank;
(5) aldehyde is dewatered in treating tower by overhead extraction product furfural, aldehyde mud is released by tower reactor, aldehyde mud delivers in recovery tower the furfural reclaimed in aldehyde mud, aldehyde mud is discharged by the bottom of tower after reclaiming furfural by recovery tower, remaining aldehyde slag is back in the hydrolysis kettle in furfural production hydrolyzing process, accomplishes to recycle without outer row completely.
The present invention with light packsly to be put except the Light ends anhydrated in aldehyde decreases the concentration of the Light ends in primary tower by de-, improves primary tower efficiency and decreases condensation reaction, reduce the Light ends of furfural; Improve thick aldehyde (1.5%), decrease Light ends, in the interference for the treatment of process, improve refining rate, Light ends is reclaimed reduces environmental pollution; Utilize water washing device to replace adding alkali neutralization, remove the organic acid in thick aldehyde, improve refining rate 4%, add economic benefit, primary tower waste water aldehyde contenting amount can be reduced simultaneously, reduce environmental pollution; Regularly reclaimed the furfural in aldehyde liquid by aldehyde mud retrieving arrangement, solve the loss that existing raffinate takes the bad recovery of furfural out of, in the foreshot of generation of simultaneously dewatering, furfural is reclaimed, and reduces in Furfural Treating Process and loses, improve furfural yield 5-6%.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the structural representation of the tower continuous treater of furfural production six of the present invention.
1 primary tower, 2 dehydration towers, 3 treating towers, 4 original fluid containers, 5 primary tower overhead condensers, 6 points of aldehyde tanks, 7 water wash columns, 8 lightness-removing columns, 9 water coolers, 10 lightness-removing column overhead condensers, 11 dehydration column overhead condensers, 12 water aldehyde tanks, 13 recycle-water aldehyde tanks, 14 recovery towers in figure.
Embodiment
As shown in the figure, the tower continuous treater of a kind of furfural production six, form primarily of primary tower 1, dehydration tower 2 and treating tower 3, increase de-with light packsly to put, water washing device and aldehyde mud retrieving arrangement, de-with light packs putting comprises lightness-removing column 8, water cooler 9 and lightness-removing column overhead condenser 10, the outlet of lightness-removing column 8 tower reactor is connected with primary tower 1 by water cooler 9, and lightness-removing column 8 tower top is connected with lightness-removing column overhead condenser 10; Water washing device comprises point aldehyde tank 6 and water wash column 7, aldehyde tank 6 top is divided to be connected with primary tower overhead condenser 5, divide bottom aldehyde tank 6 and be connected with the import of water wash column 7 tower top, divide in the middle part of aldehyde tank 6 and be connected with lightness-removing column 8 opening for feed, water wash column 7 tower top outlet is also connected with lightness-removing column 8 opening for feed, water wash column 7 outlet at bottom is connected with dehydration tower 8 import, connects a back with water inlet line bottom water wash column 7; Aldehyde mud retrieving arrangement comprises water aldehyde tank 12, recycle-water aldehyde tank 13 and recovery tower 14, water aldehyde tank 12 top is connected with dehydration column overhead condenser 11, be connected with lightness-removing column 8 opening for feed with recycle-water aldehyde tank 13 respectively bottom water aldehyde tank 12, be connected with recovery tower 14 top inlet together with bottom treating tower 3 bottom recycle-water aldehyde tank 13.Primary tower 1, dehydration tower 2 and treating tower 3 all adopt valve tray column; Lightness-removing column 8, water wash column 7 and recovery tower 14 are sieve-tray tower.
The furfural treatment technique of the tower continuous treater of above-mentioned furfural production six, by de-with light packs putting, the light constituents such as methanol acetone are separated from water aldehyde, remove the organic acid in thick aldehyde by water washing device, regularly reclaimed the furfural in aldehyde liquid by aldehyde mud retrieving arrangement, concrete technology step is as follows:
(1) rare aldehyde hydrolyzed solution enters primary tower 1 by original fluid container 4, and discharge containing high boiling material waste water at the bottom of tower, overhead vapours is condensate in layering in point aldehyde tank 6 through primary tower overhead condenser 5;
(2) dividing the aqueous phase of layering in aldehyde tank 6 to enter lightness-removing column 8, to enter lightness-removing column 8 together with the aqueous phase of water wash column 7 tower top and the water aldehyde at dehydration tower 2 top de-light, aqueous phase at the bottom of lightness-removing column 8 tower returns primary tower 1 and refluxes after water cooler 9, extraction Light ends after the condensation of lightness-removing column 8 overhead vapours, part overhead condensation liquid is back in lightness-removing column 8 simultaneously;
(3) divide the aldehyde bottom aldehyde tank 6 to enter water wash column 7 by water wash column 7 top, intake bottom water wash column 7, aldehyde water is than being 1:1, and water wash column 7 tower top aqueous phase removes lightness-removing column 8, and aldehyde at the bottom of water wash column 7 tower send dehydration tower 2 to dewater mutually;
(4) dehydration tower 2 tower top deviates from light fraction, dehydration aldehyde is discharged by dehydration tower 2 tower reactor, dehydration aldehyde send treating tower 3 to refine, light fraction enters water aldehyde tank 12 through dehydration column overhead condenser 11 condensation, after material layering in water aldehyde tank 12, it is de-light that upper materials enters lightness-removing column 8, and lower floor's material removes the furfural in recovery tower 14 in recycle-water aldehyde through recycle-water aldehyde tank 13;
(5) aldehyde is dewatered in treating tower 3 by overhead extraction product furfural, aldehyde mud is released by tower reactor, aldehyde mud delivers in recovery tower 14 furfural reclaimed in aldehyde mud, aldehyde mud is discharged by the bottom of tower after reclaiming furfural by recovery tower 14, remaining aldehyde slag is back in the hydrolysis kettle in furfural production hydrolyzing process, accomplishes to recycle without outer row completely.
Claims (3)
1. the tower continuous treater of furfural production six, form primarily of primary tower, dehydration tower and treating tower, it is characterized in that increasing de-with light packsly to put, water washing device and aldehyde mud retrieving arrangement, de-with light packs putting comprises lightness-removing column, water cooler and lightness-removing column overhead condenser, the outlet of lightness-removing column tower reactor is connected with primary tower by water cooler, and lightness-removing column tower top is connected with lightness-removing column overhead condenser; Water washing device comprises point aldehyde tank and a water wash column, aldehyde tank top is divided to be connected with primary tower overhead condenser, aldehyde pot bottom is divided to be connected with the import of water wash column tower top, divide in the middle part of aldehyde tank and be connected with lightness-removing column opening for feed, water wash column tower top outlet is also connected with lightness-removing column opening for feed, water wash column outlet at bottom is connected with dehydration tower import, connects a back with water inlet line bottom water wash column; Aldehyde mud retrieving arrangement comprises water aldehyde tank, recycle-water aldehyde tank and recovery tower, water aldehyde tank top is connected with dehydration column overhead condenser, water aldehyde pot bottom is connected with lightness-removing column opening for feed with recycle-water aldehyde tank respectively, and recycle-water aldehyde pot bottom is connected with recovery tower top inlet together with bottom treating tower.
2. the tower continuous treater of furfural production six according to claim 1, is characterized in that primary tower, dehydration tower and treating tower all adopt valve tray column; Lightness-removing column, water wash column and recovery tower are sieve-tray tower.
3. the furfural treatment technique of the tower continuous treater of furfural production six according to claim 1, it is characterized in that by de-with light packs putting, the light constituents such as methanol acetone being separated from water aldehyde, the organic acid in thick aldehyde is removed by water washing device, regularly reclaimed the furfural in aldehyde liquid by aldehyde mud retrieving arrangement, concrete technology step is as follows:
(1) rare aldehyde hydrolyzed solution enters primary tower by original fluid container, and discharge containing high boiling material waste water at the bottom of tower, overhead vapours is condensate in layering in point aldehyde tank through primary tower overhead condenser;
(2) dividing the aqueous phase of layering in aldehyde tank to enter lightness-removing column, to enter lightness-removing column together with the aqueous phase of water wash column tower top and the water aldehyde at dehydration tower top de-light, aqueous phase at the bottom of lightness-removing column tower returns primary tower and refluxes after water cooler, extraction Light ends after the condensation of lightness-removing column overhead vapours, part overhead condensation liquid is back in lightness-removing column simultaneously;
(3) divide the aldehyde of aldehyde pot bottom to enter water wash column by water wash column top, intake bottom water wash column, aldehyde water is than being 1:1, and water wash column tower top aqueous phase removes lightness-removing column, and aldehyde at the bottom of water wash column tower send dehydration tower to dewater mutually;
(4) dehydration column overhead deviates from light fraction, dehydration aldehyde is discharged by dehydration tower tower reactor, dehydration aldehyde send treating tower to refine, light fraction enters water aldehyde tank through dehydration column overhead condenser condenses, after material layering in water aldehyde tank, it is de-light that upper materials enters lightness-removing column, and lower floor's material removes the furfural in recovery tower in recycle-water aldehyde through recycle-water aldehyde tank;
(5) aldehyde is dewatered in treating tower by overhead extraction product furfural, aldehyde mud is released by tower reactor, aldehyde mud delivers in recovery tower the furfural reclaimed in aldehyde mud, aldehyde mud is discharged by the bottom of tower after reclaiming furfural by recovery tower, remaining aldehyde slag is back in the hydrolysis kettle in furfural production hydrolyzing process, accomplishes to recycle without outer row completely.
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| 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 |
| CN105330624A (en) * | 2015-11-24 | 2016-02-17 | 肥城金威机械有限公司 | Furfural refining device and method based on avoidance of neutralization reaction |
| CN105481803B (en) * | 2016-01-07 | 2018-02-16 | 唐山宏文有机肥料有限公司 | The technique and device of the semicontinuous refined furfural of continuous washing |
| CN105524031A (en) * | 2016-01-07 | 2016-04-27 | 唐山宏文有机肥料有限公司 | Process and apparatus for four-tower continuous refining of furfural |
| CN107954957A (en) * | 2017-10-30 | 2018-04-24 | 肥城金塔机械有限公司 | For producing the distilling apparatus and method of furfural |
| CN111943918A (en) * | 2020-08-24 | 2020-11-17 | 宁夏宏民生物科技有限公司 | Five-tower continuous rectification process for furfural |
| CN112174997B (en) * | 2020-09-30 | 2022-04-22 | 中国科学院过程工程研究所 | Device and method for preparing high-purity gamma-chloropropyltrichlorosilane |
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| CN102675265A (en) * | 2012-05-31 | 2012-09-19 | 天津大学 | Method of refining furfural through six-tower continuous rectification |
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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 |
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| CN102675265A (en) * | 2012-05-31 | 2012-09-19 | 天津大学 | Method of refining furfural through six-tower continuous rectification |
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| 《糠醛生产无塔式连续精制新工艺》;李晓彤等;《山西化工》;19981231(第2期);45-46 * |
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