CN104130224A - Six-tower type continuous refining device for furfural production and furfural refining process thereof - Google Patents

Six-tower type continuous refining device for furfural production and furfural refining process thereof Download PDF

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Publication number
CN104130224A
CN104130224A CN201410399151.9A CN201410399151A CN104130224A CN 104130224 A CN104130224 A CN 104130224A CN 201410399151 A CN201410399151 A CN 201410399151A CN 104130224 A CN104130224 A CN 104130224A
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Prior art keywords
tower
aldehyde
water
furfural
lightness
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CN201410399151.9A
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CN104130224B (en
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杨晓静
杨崇广
陈长君
赵强
张亚静
杨会桐
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HEBEI ZHONGKE ZHILIAN ENERGY SAVING TECHNOLOGY AG
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HEBEI ZHONGKE ZHILIAN ENERGY SAVING TECHNOLOGY AG
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/02Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
    • C07D307/34Heterocyclic 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
    • C07D307/38Heterocyclic 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
    • C07D307/40Radicals substituted by oxygen atoms
    • C07D307/46Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
    • C07D307/48Furfural

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The invention relates to a six-tower type continuous refining device for furfural production and a furfural refining process thereof. The device mainly comprises a primary tower, a dehydrating tower and a refining tower, wherein a light component removing device, a washing device and an aldehyde mud recovery device are arranged; the light component removing device comprises a light component removing tower, a cooler and a light component removing tower overhead condenser; the washing device comprises an aldehyde separating tank and a washing tower; the aldehyde mud recovery device comprises a water aldehyde tank, a recycled water aldehyde tank and a recovery tower. The device disclosed by the invention has the advantages that light components in water aldehyde are removed through the light component removing device and the concentration of the light components in the primary tower is reduced, so that the efficiency and the refining rate of the primary tower are increased; organic acid in crude aldehyde is removed by utilizing the washing device rather than alkali neutralization, so that the refining rate is increased by 4%, the economic benefit is increased, the content of aldehyde in wastewater of the primary tower is reduced and the environmental pollution is reduced; furfural in aldehyde liquid is recovered regularly through the aldehyde mud recovery device, so that the loss that the furfural carried by residual liquid is not easy to recover in the prior art is solved, in the meantime, the furfural in front fraction produced by dehydration is recovered, the loss in the furfural refining process is reduced and the furfural yield is increased by 5-6%.

Description

The tower continuous treater of furfural production six and furfural treatment technique thereof
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, hydrolysis, 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 further furfural is produced in dehydration.
2, refining, rare furfural hydrolysis liquid fractionation by distillation that hydrolysis is obtained is refining, removes in hydrolyzed solution institute 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 hydrolysis, obtains qualified finished product furfural.
The rapider ultimate production of China's furfurol industry development accounted for the 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, 5000 tons of above factories of annual output scale are a lot, the purchasing price of corn cob improves constantly, the height of furfural yield directly affects furfural production cost, to improve yield in order making rational use of resources and to reduce consumption raising quality, each factory updates technique, aspect the rectification flow of thick aldehyde, in succession using different process especially, rectification flow changes three tower continuous rectifications into by junior one tower one still technical process, three-tower type continuous refining process flow process, it is primary tower, dehydration tower, treating tower.
In current China furfural production, FF mostly adopts three tower continuous treatings or process for refining intermittently, but in treating process, light component does not separate participates in refining whole process, centre also will add rice bran water aldehyde liquid and take away a large amount of furfural foreshots 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, to solve furfural loss that prior art exists than the problem of the refining rate of considerable influence.
The tower continuous treater of furfural production six of the present invention is mainly made up of primary tower, dehydration tower and treating tower, solve technical scheme that its technical problem adopts and be increase de-with light packsly 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, divide aldehyde tank top to be connected with primary tower overhead condenser, divide aldehyde pot bottom to be connected with the import of water wash column tower top, divide aldehyde tank middle part to 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, and water wash column bottom connects a back with water inlet line; 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 treating tower bottom.
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 above-mentioned furfural production six tower continuous treaters, 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 reclaim 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, at the bottom of tower, discharges and contains high boiling material waste water, and overhead vapours is condensate in layering in point aldehyde tank through primary tower overhead condenser;
(2) dividing the water of layering in aldehyde tank to enter lightness-removing column, to enter lightness-removing column together with the water of water wash column tower top and the water aldehyde at dehydration tower top de-light, at the bottom of lightness-removing column tower, water returns to primary tower and refluxes after water cooler, the light component of extraction 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, the water inlet of water wash column bottom, aldehyde water is than being 1:1, and water wash column tower top water removes lightness-removing column, and at the bottom of water wash column tower, aldehyde send dehydration tower dehydration mutually;
(4) dehydration column overhead is deviate from light fraction, discharge dehydration aldehyde by dehydration tower tower reactor, dehydration aldehyde send treating tower refining, 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 recycle-water aldehyde in recovery tower through recycle-water aldehyde tank;
(5) dehydration aldehyde in treating tower by overhead extraction product furfural, emit aldehyde mud by tower reactor, aldehyde mud is delivered to and in recovery tower, is reclaimed the furfural in aldehyde mud, aldehyde mud is reclaimed after furfural by discharging at the bottom of tower by recovery tower, last aldehyde slag is back in the hydrolysis kettle in furfural production hydrolyzing process, accomplishes to recycle without outer row completely.
The present invention, by the de-with light packs concentration that has reduced the light component in primary tower except the light component anhydrating in aldehyde of putting, has improved primary tower efficiency and has reduced condensation reaction, reduces the light component of furfural; Improve thick aldehyde (1.5%), reduced light component, in the interference for the treatment of process, improved refining rate, light component is reclaimed reduces environmental pollution; Utilize water washing device to replace and add alkali neutralization, remove the organic acid in thick aldehyde, improved refining rate 4%, increased economic benefit, can reduce primary tower waste water aldehyde contenting amount, reduce environmental pollution simultaneously; Regularly reclaim the furfural in aldehyde liquid by aldehyde mud retrieving arrangement, solve existing raffinate and take out of the loss of the bad recovery of furfural, in the foreshot that dehydration produces simultaneously, furfural is reclaimed, and reduces in Furfural Treating Process and loses, and has improved furfural yield 5-6%.
Brief description of the drawings
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the structural representation of furfural production six tower continuous treaters of the present invention.
1 primary tower in figure, 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.
Embodiment
As shown in the figure, the tower continuous treater of a kind of furfural production six, mainly formed by primary tower 1, dehydration tower 2 and treating tower 3, increase de-with light packsly 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, lightness-removing column 8 tower reactor outlets are connected with primary tower 1 by water cooler 9, and lightness-removing column 8 tower tops are connected with lightness-removing column overhead condenser 10; Water washing device comprises point aldehyde tank 6 and water wash column 7, divide aldehyde tank 6 tops to be connected with primary tower overhead condenser 5, divide aldehyde tank 6 bottoms to be connected with water wash column 7 tower top imports, divide aldehyde tank 6 middle parts to be connected with lightness-removing column 8 opening for feeds, water wash column 7 tower top outlets are also connected with lightness-removing column 8 opening for feeds, water wash column 7 outlet at bottoms are connected with dehydration tower 8 imports, and water wash column 7 bottoms connect a back with water inlet line; Aldehyde mud retrieving arrangement comprises water aldehyde tank 12, recycle-water aldehyde tank 13 and recovery tower 14, water aldehyde tank 12 tops are connected with dehydration column overhead condenser 11, water aldehyde tank 12 bottoms are connected with lightness-removing column 8 opening for feeds with recycle-water aldehyde tank 13 respectively, and recycle-water aldehyde tank 13 bottoms are connected with recovery tower 14 top inlet together with treating tower 3 bottoms.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 above-mentioned furfural production six tower continuous treaters, 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 reclaim 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, at the bottom of tower, discharges and contains high boiling material waste water, and overhead vapours is condensate in layering in point aldehyde tank 6 through primary tower overhead condenser 5;
(2) dividing the water of layering in aldehyde tank 6 to enter lightness-removing column 8, to enter lightness-removing column 8 together with the water of water wash column 7 tower tops and the water aldehyde at dehydration tower 2 tops de-light, at the bottom of lightness-removing column 8 towers, water returns to primary tower 1 and refluxes after water cooler 9, the light component of extraction after lightness-removing column 8 overhead vapours condensations, part overhead condensation liquid is back in lightness-removing column 8 simultaneously;
(3) divide the aldehyde of aldehyde tank 6 bottoms to enter water wash column 7 by water wash column 7 tops, water wash column 7 bottom water inlets, aldehyde water is than being 1:1, and water wash column 7 tower top waters remove lightness-removing column 8, and at the bottom of water wash column 7 towers, aldehyde send dehydration tower 2 to dewater mutually;
(4) dehydration tower 2 tower tops are deviate from light fraction, discharge dehydration aldehyde by dehydration tower 2 tower reactors, dehydration aldehyde send treating tower 3 refining, light fraction enters water aldehyde tank 12 through 11 condensations of dehydration column overhead condenser, 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 recycle-water aldehyde in recovery tower 14 through recycle-water aldehyde tank 13;
(5) dehydration aldehyde in treating tower 3 by overhead extraction product furfural, emit aldehyde mud by tower reactor, aldehyde mud is delivered to and in recovery tower 14, is reclaimed the furfural in aldehyde mud, aldehyde mud is reclaimed after furfural by discharging at the bottom of tower by recovery tower 14, last 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, mainly formed by primary tower, dehydration tower and treating tower, it is characterized in that increasing de-with light packsly 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, divide aldehyde tank top to be connected with primary tower overhead condenser, divide aldehyde pot bottom to be connected with the import of water wash column tower top, divide aldehyde tank middle part to 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, and water wash column bottom connects a back with water inlet line; 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 treating tower bottom.
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 exquisite technique of the furfural of furfural production six tower continuous treaters claimed in 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, remove the organic acid in thick aldehyde by water washing device, regularly reclaim 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, at the bottom of tower, discharges and contains high boiling material waste water, and overhead vapours is condensate in layering in point aldehyde tank through primary tower overhead condenser;
(2) dividing the water of layering in aldehyde tank to enter lightness-removing column, to enter lightness-removing column together with the water of water wash column tower top and the water aldehyde at dehydration tower top de-light, at the bottom of lightness-removing column tower, water returns to primary tower and refluxes after water cooler, the light component of extraction 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, the water inlet of water wash column bottom, aldehyde water is than being 1:1, and water wash column tower top water removes lightness-removing column, and at the bottom of water wash column tower, aldehyde send dehydration tower dehydration mutually;
(4) dehydration column overhead is deviate from light fraction, discharge dehydration aldehyde by dehydration tower tower reactor, dehydration aldehyde send treating tower refining, 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 recycle-water aldehyde in recovery tower through recycle-water aldehyde tank;
(5) dehydration aldehyde in treating tower by overhead extraction product furfural, emit aldehyde mud by tower reactor, aldehyde mud is delivered to and in recovery tower, is reclaimed the furfural in aldehyde mud, aldehyde mud is reclaimed after furfural by discharging at the bottom of tower by recovery tower, last aldehyde slag is back in the hydrolysis kettle in furfural production hydrolyzing process, accomplishes to recycle without outer row completely.
CN201410399151.9A 2014-08-14 2014-08-14 The tower continuous treater of furfural production six and furfural treatment technique thereof Expired - Fee Related CN104130224B (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN105481803A (en) * 2016-01-07 2016-04-13 唐山宏文有机肥料有限公司 Technology and device for continuously washing and semi-continuously refining furfural
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
CN112174997A (en) * 2020-09-30 2021-01-05 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
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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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN105481803A (en) * 2016-01-07 2016-04-13 唐山宏文有机肥料有限公司 Technology and device for continuously washing and semi-continuously refining furfural
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
CN112174997A (en) * 2020-09-30 2021-01-05 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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