CN105198842A - Clean production line for furfural and production method of furfural - Google Patents
Clean production line for furfural and production method of furfural Download PDFInfo
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- CN105198842A CN105198842A CN201510692527.XA CN201510692527A CN105198842A CN 105198842 A CN105198842 A CN 105198842A CN 201510692527 A CN201510692527 A CN 201510692527A CN 105198842 A CN105198842 A CN 105198842A
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- aldehyde
- furfural
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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
- C07D307/50—Preparation from natural products
Abstract
The invention discloses a clean production line for furfural and a production method of the furfural. The clean production line comprises process facilities for sieving, crushing, acid preparation, hydrolysis, prefractionation, separation, rectification and the like and also further comprises treatment facilities for waste gas, wastewater and waste slag. The hydrolysis refers to charging corncobs mixed with acid to a hydrolysis pot at a charging density of 0.18 to 0.2t/m<3>, wherein the steam pressure is 0.5 to 1.0 MPa and the steam temperature is 140 to 180 DEG C in the hydrolysis pot; the tower top temperature is 94 to 97 DEG C and the tower bottom temperature is 98 to 108 DEG C in a prefractionation tower, furfural-containing water vapor is discharged from the tower top, and is condensed into liquid through a condenser, the liquid then enters a furfural separation tank to be subjected to water-furfural separation, and furfural liquid about 90 to 93% at the bottom automatically flows to a raw furfural tank. The clean production line disclosed by the invention can be used for scale processing of corncobs, and a separation effect of acetic acid and water can reach an international advanced level.
Description
Technical field
The present invention relates to production unit and the technological process of production thereof of producing furfuryl aldehyde solution with the waste of agricultural-food.
Background technology
Furfural has another name called furtural, is water white liquid, has amygdaloid smell, flash-point 60 DEG C, fusing point-36.5 DEG C, boiling point 161.7 DEG C.Be dissolved in hot water, ethanol, ether and benzene, oxidation gradually becomes yellow to brown in atmosphere.
At present, the furfural production of China is mainly raw material with corn cob, and take sulfuric acid as catalyzer, single stage method is produced.Furfural production adopts pressurized hydrolysis production technique, and main process comprises: cleaning, raw material pulverizing, nitration mixture, hydrolysis, condensation, fore-running, separation and rectifying etc.
But the rate of output and three-protection design etc. have much room for improvement.
Hydrolysis principal reaction equation is as follows:
Number of patent application is a kind of furfural production and waste water, waste residue, the off gas treatment integral process of 2009100102714, is applicable to furfural production industry energy conservation and three-protection design transformation.It is characterized in that adopting in Wingdale and rhombspar and furfural waste-water, make acetic acid be converted into calcium magnesium acetate, the high temperature aldehyde vapour heat exchange then produced with hydrolyzer, then enter vaporizer; The high-temperature vapor that waste water evaporation produces enters hydrolyzer as reaction medium, and extract calcium acetate magnesium salt after the decolouring of residue concentrated solution, raffinate is used for flue gas desulfurization, denitration.High temperature aldehyde slag reclaims after furfural from thermal evaporation through low pressure, then makes aldehyde slag water ratio be down to less than 20% through cryodrying.Though the three wastes of this invention have better process, but the auxiliary material used is more, and cost is higher, and the aftertreatment of waste water comparatively bothers.
Number of patent application a kind of corn cob that has been the disclosure of the invention of 2012100966677 produces the production method of furfural, its step is, first corn cob is pulverized and dilute sulphuric acid mixing, then through hydrolysis treatment, then the furfural steam obtained carry out removal of impurities operation through neutralization, again through repeated multiple times distillation, in the collector of furfural steam income condenser, then the chaff aldehyde obtained again through neutralizing treatment, then carry out refining obtaining final furfural goods with distillation under vacuum or steam distillation.This invention is to treatment process parameter insufficient disclosure, and be difficult to Guiding Practice, waste water reclamation utilizes not good enough.
Number of patent application be 2011101067039 invention to relate to a kind of take corn cob as the method that furfural prepared by raw material.Said method comprising the steps of: after 1) being pulverized by corn cob, the sulphuric acid soln being 0.1 ~ 0.5wt% with concentration mixes; 2) by step 1) in mixture heating, add additive phenols and fragrant amine polymerization inhibitor, be uniformly mixed; Wherein the add-on of additive accounts for corn cob total mass 0.05 ~ 0.5%; 3) in corn cob hydrolytic reaction pot, there is hydrolysis reaction generate furfural, the middle part of described reactor is provided with wire dividing plate, by step 2) in join on the wire dividing plate in corn cob hydrolytic reaction pot containing the mixture of additive, hydrolysis temperature is 150 ~ 190 DEG C, water rear rising, contacts with mixture, and hydrolysis reaction occurs, the hydrolysate furfural effusion of gaseous state, obtains furfural phlegma.Containing the by product that other additive brings in the finished product of this invention.
Summary of the invention
Goal of the invention:
The invention provides a kind of reaction product purity is high, three waste discharge is few furfural cleaner production streamline and production method thereof.
Technical scheme:
Furfural cleaner production streamline provided by the invention and production method thereof, have: process facility and the processing steps thereof such as screening, pulverizing, complex acid, hydrolysis, fore-running, separation and rectifying, separately have the treatment facility of waste gas, waste water and waste residue.Preferably there is self-con-tained unit, system-wide Automated condtrol production process can be realized.
Wherein,
Screening: corn cob is mixed with the foreign material such as silt unavoidably, isolates dust impurity in screening process.
Pulverize and charging: corn cob transports to crushing section by screw feeder, and the corn cob granularity after pulverizing is about 10-20mm, and particle wind delivers to closed feed bin.
Nitration mixture: the vitriol oil is made into the preferred 2-4% of 2 ~ 6%(, better to degradation effect) dilute sulphuric acid, to be added in acid mixer after valve regulated metering, and raw material Homogeneous phase mixing, to accomplish that raw material and diluted acid add simultaneously.
Hydrolysis: produce wood sugar by the pentosan be rich in corn cob, wood sugar generates furfural after dehydration.Hydrolysis is carried out in hydrolyzer, by the loading density of 0.18-0.2t/m3, the corn cob after nitration mixture is loaded hydrolyzer, cover pot cover, steam is sent to enter sweating room at the bottom of tank after screwing, start the pressurization that heats up, the time of whole hydrolysis is about 4-6 hour, and the vapor pressure in hydrolyzer is the preferred 0.6-0.8MPa of 0.5-1.0MPa(), vapor temperature is 140-180 DEG C (preferred 160-175 DEG C), the rate of output that is most effective, hydrolysis of now corn cob hydrolysis is best.The hair aldehyde gas azeotrope generated after reaction discharges (now furfural content about 5%) by tower top pipeline, and hydrolysis residue is drained bottom hydrolyzer.
Fore-running: enter primary tower from hydrolyzer hair aldehyde gas out after cooling, Secondary-steam heating concentrate is used bottom primary tower, (first to pass in automatic steam control tower temperature at 65-80 DEG C, tower top temperature remains on 55-70 DEG C, the time of this temperature range is kept to be the 1/3-1/2 of whole fore-running heat-up time, slow heating makes moisture and furfural sepn process slow down, and active principle runs off and reduces).Continue to distill aldehyde liquid, raise temperature in tower, make furfural water system azeotropic vaporization, maintenance tower top temperature is 94-97 DEG C, and column bottom temperature is 98-108 DEG C, tower top is discharged containing aldehyde steam, become liquid containing aldehyde steam through condenser condenses and enter a point aldehyde tank, utilize proportion difference (water=1, furfural=1.16), in point aldehyde tank, water aldehyde is separated, divide aldehyde tank top containing the aqueous solution of aldehyde about 7%-10%, be back to primary tower and evaporate again.The aldehyde liquid of bottom about 90%-93% flows automatically to a mao aldehyde tank.Bottom primary tower, waste water is delivered to sewage treatment plant and is processed.
Neutralization: hair aldehyde enters neutralization tank after metering, with alkali-prepared tank come the dilute soda aqueous solution stirs in neutralization tank in, sodium-acetate, water and carbonic acid gas is generated with the acetic acid reaction in hair aldehyde, the separation of water aldehyde is carried out further through hair aldehyde setting tank after neutralization, ensure that most of moisture is separated discharge as early as possible, the secondary aldehyde liquid after water aldehyde is separated discharges rectifying tower from tower bottom again.
Rectifying: rectifying tower internal pressure controls at about negative pressure 0.07-0.09MPa, in control tower, temperature is at 105-110 DEG C simultaneously, and tower top temperature remains on 95-100 DEG C.Furfural with this understanding in material is distilled out of, and furfural steam obtains the furfural finished product of concentration more than 99% after condensation, squeezes into finished pot.
Aldehyde mud bottom treating tower (be mainly that formic acid is received, sodium-acetate and a small amount of water) recycles separately.
Beneficial effect:
This invention can be used in the extensive process of corn ear, and the time of hydrolysis, fore-running, dehydration, rectifying, temperature and pressure arrange rationally, and the purity of gained finished product furfural is high, and the rate of output is high.Water-vapor quality makes full use of, and energy consumption is lower, and waste water,waste gas and industrial residue meets environmental requirement.
Detect through GC, the separating effect of Sn-ZSM-5 zeolite molecular sieve film to acetic acid/water fullys meet international most advanced level, it is feasible for illustrating that Sn-ZSM-5 zeolite molecular sieve film is applied in the application of acetic acid in pervaporation recovery furfural waste-water, has important industrial application value.
Accompanying drawing explanation
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Furfural cleaner production streamline as shown in Figure 1, has the process facility of screening, pulverizing, complex acid, hydrolysis, fore-running, separation and rectifying, separately has the reprocessing facility of waste gas, waste water and waste residue.
In nitration mixture processing step, be the vitriol oil is made into 3 ~ 5% dilute sulphuric acid, and raw material corn cob Homogeneous phase mixing, raw material and diluted acid add simultaneously;
In hydrolysis process step: by the loading density of 0.18-0.2t/m3, the corn cob after nitration mixture is loaded hydrolyzer, the time of whole hydrolysis is 4-6 hour, vapor pressure in hydrolyzer is 0.5-1.0MPa, vapor temperature is 150-170 DEG C, the hair aldehyde gas azeotrope generated after hydrolysis reaction is discharged by tower top pipeline, and hydrolysis residue is discharged and carried out aftertreatment bottom hydrolyzer.
Fore-running: enter primary tower from hydrolyzer hair aldehyde gas out after cooling, use Secondary-steam heating concentrate bottom primary tower, first passes in automatic steam control tower that temperature is at 70-80 DEG C, and tower top temperature remains on 60-70 DEG C.Top, containing the aqueous solution of aldehyde about 7%-10%, is back to primary tower and evaporates.Then, continue to raise temperature in tower, make furfural water system azeotropic vaporization, maintenance tower top temperature is 94-97 DEG C, and column bottom temperature is 98-108 DEG C, and tower top is discharged containing aldehyde steam, become liquid containing aldehyde steam through condenser condenses and enter a point aldehyde tank, utilize proportion different, in point aldehyde tank, water aldehyde is separated; The hair aldehyde liquid of bottom flows automatically to a mao aldehyde tank.
Neutralization: hair aldehyde liquid enters neutralization tank after metering again, with alkali-prepared tank come the dilute soda aqueous solution stirs in neutralization tank in, generate sodium-acetate, water and carbonic acid gas with the acetic acid reaction in hair aldehyde liquid, after neutralization, carry out the separation of water aldehyde further through hair aldehyde setting tank again.
Rectifying: the secondary aldehyde liquid after water aldehyde is separated sends into rectifying tower, and rectifying tower internal pressure controls at about negative pressure 0.07-0.09MPa, in control tower, temperature is at 105-110 DEG C simultaneously, and tower top temperature remains on 95-100 DEG C; Furfural with this understanding in material is distilled out of, and furfural steam squeezes into finished pot after condensation.
Claims (4)
1. a furfural cleaner production streamline, has screening, pulverizing, complex acid, hydrolysis, fore-running, the process facility of separation and rectifying and processing step thereof, it is characterized in that: the reprocessing facility separately with waste gas, waste water and waste residue;
In nitration mixture processing step, be the vitriol oil is made into 2 ~ 6% dilute sulphuric acid, and raw material corn cob Homogeneous phase mixing, raw material and diluted acid add simultaneously;
In hydrolysis process step: by the loading density of 0.18-0.2t/m3, the corn cob after nitration mixture is loaded hydrolyzer, the time of whole hydrolysis is 4-6 hour, vapor pressure in hydrolyzer is 0.5-1.0MPa, vapor temperature is 140-180 DEG C, the hair aldehyde gas azeotrope generated after hydrolysis reaction is discharged by tower top pipeline, and hydrolysis residue is discharged and carried out aftertreatment bottom hydrolyzer;
Fore-running: enter primary tower from hydrolyzer hair aldehyde gas out after cooling, Secondary-steam heating concentrate is used bottom primary tower, raise temperature in tower, make furfural water system azeotropic vaporization, maintenance tower top temperature is 94-97 DEG C, and column bottom temperature is 98-108 DEG C, tower top is discharged containing aldehyde steam, become liquid containing aldehyde steam through condenser condenses and enter a point aldehyde tank, utilize proportion different, in point aldehyde tank, water aldehyde is separated; The hair aldehyde liquid of bottom flows automatically to a mao aldehyde tank;
Neutralization: hair aldehyde liquid enters neutralization tank after metering again, with alkali-prepared tank come the dilute soda aqueous solution stirs in neutralization tank in, generate sodium-acetate, water and carbonic acid gas with the acetic acid reaction in hair aldehyde liquid, after neutralization, carry out the separation of water aldehyde further through hair aldehyde setting tank again;
Rectifying: the secondary aldehyde liquid after water aldehyde is separated sends into rectifying tower, and rectifying tower internal pressure controls at about negative pressure 0.07-0.09MPa, in control tower, temperature is at 105-110 DEG C simultaneously, and tower top temperature remains on 95-100 DEG C; Furfural with this understanding in material is distilled out of, and furfural steam squeezes into finished pot after condensation.
2. furfural cleaner production streamline water aldehyde as claimed in claim 1 is separated, it is characterized in that: in primary tower, first pass in automatic steam control tower that temperature is at 65-80 DEG C, tower top temperature remains on 55-70 DEG C, keeps the time of this temperature range to be the 1/3-1/2 of whole fore-running heat-up time.
3. furfural cleaner production streamline water aldehyde as claimed in claim 1 is separated, and it is characterized in that: point aldehyde tank top, containing the aqueous solution of aldehyde about 7%-10%, is back to primary tower and evaporates.
4. furfural cleaner production streamline water aldehyde as claimed in claim 1 or 2 is separated, and it is characterized in that: bottom primary tower, waste water is delivered to sewage treatment plant and processed.
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| CN201510692527.XA CN105198842A (en) | 2015-10-23 | 2015-10-23 | Clean production line for furfural and production method of furfural |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107721952A (en) * | 2017-11-25 | 2018-02-23 | 宁津春蕾生物科技有限公司 | furfural preparation technology |
| CN108314666A (en) * | 2017-01-17 | 2018-07-24 | 沈阳市利农秸杆燃料开发有限公司 | The method for producing furfural using stalk |
| CN108929291A (en) * | 2017-05-23 | 2018-12-04 | 宁津春蕾生物科技有限公司 | The production technology of furfural |
| CN109589638A (en) * | 2019-01-21 | 2019-04-09 | 山西恒宇生物科技有限公司 | A kind of furfural raffinate includes the extraction element and extraction process of aldehyde |
| CN110407780A (en) * | 2019-08-23 | 2019-11-05 | 山东省化工研究院 | A kind of refining methd of furfural |
| CN110590718A (en) * | 2019-09-06 | 2019-12-20 | 辽宁全康生物科技集团有限责任公司 | Production method for extracting furfural from corncobs |
| CN110642813A (en) * | 2019-09-09 | 2020-01-03 | 山东省化工研究院 | Preparation process 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 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108314666A (en) * | 2017-01-17 | 2018-07-24 | 沈阳市利农秸杆燃料开发有限公司 | The method for producing furfural using stalk |
| CN108929291A (en) * | 2017-05-23 | 2018-12-04 | 宁津春蕾生物科技有限公司 | The production technology of furfural |
| CN107721952A (en) * | 2017-11-25 | 2018-02-23 | 宁津春蕾生物科技有限公司 | furfural preparation technology |
| CN109589638A (en) * | 2019-01-21 | 2019-04-09 | 山西恒宇生物科技有限公司 | A kind of furfural raffinate includes the extraction element and extraction process of aldehyde |
| CN109589638B (en) * | 2019-01-21 | 2021-07-27 | 山西恒宇生物科技有限公司 | Extraction device and extraction process for aldehyde in furfural residual liquid |
| CN110407780A (en) * | 2019-08-23 | 2019-11-05 | 山东省化工研究院 | A kind of refining methd of furfural |
| CN110590718A (en) * | 2019-09-06 | 2019-12-20 | 辽宁全康生物科技集团有限责任公司 | Production method for extracting furfural from corncobs |
| CN110642813A (en) * | 2019-09-09 | 2020-01-03 | 山东省化工研究院 | Preparation process 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 |
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Application publication date: 20151230 |