CN205420242U - Furfural cleaner production assembly line - Google Patents
Furfural cleaner production assembly line Download PDFInfo
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- CN205420242U CN205420242U CN201520824287.XU CN201520824287U CN205420242U CN 205420242 U CN205420242 U CN 205420242U CN 201520824287 U CN201520824287 U CN 201520824287U CN 205420242 U CN205420242 U CN 205420242U
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Abstract
The utility model discloses a furfural cleaner production assembly line has: the screening, smash, the complex acid, hydrolysis, technology facilities such as fore -running, separation and rectification, other has the processing facility of waste gas, waste water and waste residue. Corncob feed inlet passes through the screw feeder intercommunication and smashes the workshop section, and crushing workshop section passes through pneumatic conveying device and connects the feed bin, mixes and is connected with the valve of adjusting the measurement function between sour machine and the dilute sulfuric acid inlet port, the fore -running top of the tower has including aldehyde steam discharge port, divides the aldehyde jar through the condenser intercommunication, the rectifying column has furfural steam outlet, through condensing equipment intercommunication finished product jar. The utility model discloses a purity of gained finished product furfural is high, and rate of output is high. Steam resource make full use of, the energy consumption is lower, and waste water, waste gas, waste residue accord with the environmental protection requirement.
Description
Technical field
This utility model relates to production equipment and the technological process of production thereof producing furfuryl aldehyde solution with the garbage of agricultural product.
Background technology
Furfural has another name called furtural, is water white liquid, has amygdaloid abnormal smells from the patient, flash-point 60 DEG C, fusing point-36.5 DEG C, boiling point 161.7 DEG C.Being dissolved in hot water, ethanol, ether and benzene, oxidation gradually becomes yellow to sepia in atmosphere.
At present, the furfural production of China is mainly with corn cob as raw material, and with sulphuric acid as catalyst, one-step method produces.Furfural production uses pressurized hydrolysis production technology, and main process includes: cleaning, raw material pulverizing, nitration mixture, hydrolyze, condense, fore-running, separation and rectification etc..
But, the rate of output and three-protection design etc. have much room for improvement.
Hydrolysis dominant response equation is as follows:
Number of patent application is a kind of furfural production and waste water, waste residue, the exhaust-gas treatment integral process of 2009100102714, it is adaptable to furfural production industry energy conservation and three-protection design transformation.It is characterized in that using in limestone and dolomite and furfural waste-water, make acetic acid be converted into calcium magnesium acetate, the high temperature aldehyde vapour heat exchange then produced with hydrolyzer, enter back into vaporizer；The high-temperature vapor that waste water evaporation produces enters hydrolyzer and extracts calcium acetate magnesium salt as reaction medium, residue concentrated solution after decolouring, and residual liquid is used for flue gas desulfurization, denitration.High temperature aldehyde slag is after low pressure is from thermal evaporation recovery furfural, then makes aldehyde slag moisture content be down to less than 20% through cold drying.Though the three wastes of this invention have preferably process, but the auxiliary material used is more, and relatively costly, the post processing of waste water is cumbersome.
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 sulfuric acid mixes, it is then passed through hydrolysis process, then the furfural steam obtained carry out remove impurity operation through neutralizing, again through repeated multiple times distillation, in catcher furfural steam income condenser, then the chaff aldehyde obtained is again passed by neutralisation treatment, then carry out being refining to obtain final furfural goods with distillation under vacuum or steam distillation.This invention is to processing technological parameter insufficient disclosure, it is difficult to Guiding Practice, waste water reclamation utilizes not good enough.
Summary of the invention
Utility model purpose:
This utility model provides the furfural cleaning production line and production method thereof that a kind of product purity is high, three waste discharge is few.
Technical scheme:
The furfural cleaning production line that this utility model provides, has: sieve, pulverize, complex acid, process facility (or workshop section) and the processing step thereof such as hydrolysis, fore-running, separation and rectification, separately there is the treatment facility of waste gas, waste water and waste residue.Preferably there is self-con-tained unit, it is possible to realize system-wide Automated condtrol production process.
Wherein,
Screening: corn cob is mixed with the foreign material such as silt unavoidably, isolates dust impurity in screening process.
Pulverizing and charging: corn cob transports to break section by screw(-type) feeder, the corn cob granularity about 10-20mm after pulverizing, particle wind delivers to the feed bin closed.
I.e. corn cob feed(raw material)inlet connects break section by screw(-type) feeder, and break section send device to connect feed bin by wind.
Complex acid: concentrated sulphuric acid is made into the preferred 2-4% of 2 ~ 6%(, more preferable to degradation effect) dilute sulfuric acid, be added in acid mixer after valve regulated is measured, and raw material corn cob uniformly mix, and accomplishes that raw material adds with diluted acid simultaneously.
I.e. acid mixer has dilute sulfuric acid and adds entrance and corn cob adds entrance, and acid mixer adds with dilute sulfuric acid and is connected the valve having regulation function of measuring between entrance.
Hydrolysis: by corn cob rich in pentosan produce xylose, xylose through dehydration after generate furfural.Hydrolysis is carried out in hydrolyzer, corn cob after mixing acid by the loading density of 0.18-0.2t/m3 loads hydrolyzer, cover pot cover, steam is sent to enter tank bottoms vaporium after screwing, start to warm up pressurization, the time of whole hydrolysis is about 4-6 hour, and the steam pressure in hydrolyzer is the preferred 0.6-0.8MPa of 0.5-1.0MPa(), vapor (steam) temperature be 140-180 DEG C (preferably 160-175 DEG C), now corn cob hydrolysis efficiency the highest, hydrolysis the rate of output best.The hair aldehyde gas azeotropic mixture generated after reaction is discharged (now furfural content about 5%) by hydrolyzer push pipe road, and hydrolysis residue is drained bottom hydrolyzer.
The i.e. end of hydrolyzer, has vaporium, and hydrolyzer top connects hairiness aldehyde gas discharge line, and the bottom of hydrolyzer also has hydrolysis residue outlet.
Fore-running: enter primary distillation tower after cooling from hydrolyzer hair aldehyde gas out, Secondary-steam heating concentration is used bottom primary distillation tower, (in passing first into automatic steam control primary distillation tower, temperature is at 65-80 DEG C, fore-running tower top temperature is maintained at 55-70 DEG C, the 1/3-1/2 keeping time of this temperature range to be whole fore-running heat time heating time, being slowly heated so that moisture slows down with furfural separation process, active component runs off and reduces).Continue aldehyde liquid is distilled, raise temperature in primary distillation tower, making furfural and water azeotropic vaporization, keep tower top temperature to be 94-97 DEG C, column bottom temperature is 98-108 DEG C, primary distillation tower top row goes out containing aldehyde steam, the condensation of the condensed device of the steam containing aldehyde becomes liquid and enters a point aldehyde tank, utilizes proportion different (water=1, furfural=1.16), and in point aldehyde tank, water aldehyde separates, divide the aldehyde tank top aqueous solution containing aldehyde about 7%-10%, be back to primary distillation tower and carry out re-evaporation.The hair aldehyde liquid of bottom about 90%-93% flows automatically to a mao aldehyde tank.Bottom primary distillation tower, waste water is delivered to sewage treatment plant and is processed.
Primary distillation tower entrance is connected after i.e. hair aldehyde gas discharge line connects chiller；Fore-running tower top has containing aldehyde steam outlet, by condenser connection point aldehyde tank；Divide aldehyde tank top to have the outlet containing aldehyde aqueous solution, connect primary distillation tower entrance by reflux pipe.Divide aldehyde pot bottom to have a mao outlet for aldehyde liquid, connect hair aldehyde tank.There is bottom primary distillation tower wastewater outlet, connect sewage treatment plant.
Neutralize: the hair aldehyde in hair aldehyde tank enters neutralizing tank after metering, the dilute soda aqueous solution come with alkali-prepared tank stirs neutralization in neutralizing tank, sodium acetate, water and carbon dioxide is generated with the acetic acid reaction in hair aldehyde, water aldehyde separation is carried out further through hair aldehyde settling tank after neutralization, ensureing that most of moisture separates discharge as early as possible, the secondary aldehyde liquid after water aldehyde separates discharges rectifying column from tower bottom again.
I.e. hair aldehyde tank connects neutralizing tank, neutralizing tank connection hair aldehyde settling tank by metering device, has the outlet of secondary aldehyde liquid, secondary aldehyde liquid outlet rectifying column bottom hair aldehyde settling tank.
Rectification: in rectifying column, Stress control is about negative pressure 0.07-0.09MPa, in control tower, temperature is at 105-110 DEG C simultaneously, and tower top temperature is maintained at 95-100 DEG C.Furfural in material is distilled out of with this understanding, obtains the furfural finished product of concentration more than 99%, squeeze into finished pot after furfural steam is condensed.
The aldehyde mud of rectifier bottoms (predominantly formic acid receive, sodium acetate and a small amount of water) recycles separately.
I.e. rectifying column has furfural steam (vapor) outlet, connects finished pot by condensing unit, and rectifier bottoms has the outlet of aldehyde mud.Beneficial effect:
This utility model can be used in the extensive process of corncob, and hydrolysis, fore-running, dehydration, the time of rectification, 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 relatively low, and waste water,waste gas and industrial residue meets environmental requirement.
Detect through GC, Sn-ZSM-5 zeolite molecular sieve film fullys meet international most advanced level to the separating effect of acetic acid/water, illustrating that Sn-ZSM-5 zeolite molecular sieve film is applied in pervaporation reclaims furfural waste-water is feasible in the application of acetic acid, has important industrial application value.
Accompanying drawing explanation
Fig. 1 is a process chart of the present utility model.
Fig. 2 is a process facility connection diagram of the present utility model.
Detailed description of the invention
Furfural cleaning production line as shown in accompanying drawing 1, Fig. 2, has the process facility of screening, pulverizing, complex acid, hydrolysis, fore-running, separation and rectification, separately has the reprocessing facility of waste gas, waste water and waste residue.
In nitration mixture processing step, be concentrated sulphuric acid is made into 3 ~ 5% dilute sulfuric acid, and raw material corn cob uniformly mixes, and raw material adds with diluted acid 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, steam pressure in hydrolyzer is 0.5-1.0MPa, vapor (steam) temperature is 150-170 DEG C, the hair aldehyde gas azeotropic mixture generated after hydrolysis is discharged by tower top pipeline, and hydrolysis residue is discharged bottom hydrolyzer and carried out post processing.
Fore-running: entering primary distillation tower after cooling from hydrolyzer hair aldehyde gas out, use Secondary-steam heating concentration bottom primary distillation tower, in passing first into automatic steam control tower, temperature is at 70-80 DEG C, and tower top temperature is maintained at 60-70 DEG C.The top aqueous solution containing aldehyde about 7%-10%, is back to primary distillation tower and carries out re-evaporation.Then, continue to rise temperature in high tower, make furfural and water azeotropic vaporization, keeping tower top temperature to be 94-97 DEG C, column bottom temperature is 98-108 DEG C, and tower top discharges the steam in aldehyde, the condensation of the condensed device of the steam containing aldehyde becomes liquid and enters a point aldehyde tank, utilizes proportion different, and in point aldehyde tank, water aldehyde separates；The hair aldehyde liquid of bottom flows automatically to a mao aldehyde tank.
Neutralizing: hair aldehyde liquid enters back into neutralizing tank after metering, the dilute soda aqueous solution come with alkali-prepared tank stirs neutralization in neutralizing tank, generates sodium acetate, water and carbon dioxide with the acetic acid reaction in hair aldehyde liquid, carries out water aldehyde separation further through hair aldehyde settling tank again after neutralization.
Rectification: the secondary aldehyde liquid after water aldehyde separates sends into rectifying column, and in rectifying column, Stress control is about negative pressure 0.07-0.09MPa, and in control tower, temperature is at 105-110 DEG C simultaneously, and tower top temperature is maintained at 95-100 DEG C；Furfural in material is distilled out of with this understanding, squeezes into finished pot after furfural steam is condensed.
Claims (3)
1. a furfural cleaning production line, has the process facility of screening, pulverizing, complex acid, hydrolysis, fore-running, separation and rectification, it is characterized in that: separately have the reprocessing facility of waste gas, waste water and waste residue；
Corn cob feed(raw material)inlet connects break section by screw(-type) feeder, and break section send device to connect feed bin by wind；
Acid mixer has dilute sulfuric acid and adds entrance and corn cob adds entrance, and acid mixer adds with dilute sulfuric acid and is connected the valve having regulation function of measuring between entrance；
The end of hydrolyzer, has vaporium, and hydrolyzer top connects hairiness aldehyde gas discharge line, and the bottom of hydrolyzer also has hydrolysis residue outlet；
Hair aldehyde gas discharge line connects primary distillation tower entrance after connecting chiller；Fore-running tower top has containing aldehyde steam outlet, by condenser connection point aldehyde tank；
Hair aldehyde tank connects neutralizing tank, neutralizing tank connection hair aldehyde settling tank by metering device, has the outlet of secondary aldehyde liquid, secondary aldehyde liquid outlet rectifying column bottom hair aldehyde settling tank；
Rectifying column has furfural steam (vapor) outlet, connects finished pot by condensing unit, and rectifier bottoms has the outlet of aldehyde mud.
2. furfural cleaning production line water aldehyde as claimed in claim 1 separates, and it is characterized in that: a point aldehyde tank top has the outlet containing aldehyde aqueous solution, connects primary distillation tower entrance by reflux pipe；Divide aldehyde pot bottom to have the outlet of aldehyde liquid, connect hair aldehyde tank.
3. furfural cleaning production line water aldehyde as claimed in claim 1 separates, and it is characterized in that: have wastewater outlet bottom primary distillation tower, connects sewage treatment plant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520824287.XU CN205420242U (en) | 2015-10-23 | 2015-10-23 | Furfural cleaner production assembly line |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201520824287.XU CN205420242U (en) | 2015-10-23 | 2015-10-23 | Furfural cleaner production assembly line |
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| CN205420242U true CN205420242U (en) | 2016-08-03 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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2015
- 2015-10-23 CN CN201520824287.XU patent/CN205420242U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Address after: 200434 Hongkou District Memorial Road, Hongkou District, Shanghai, room 1401, room 8 Patentee after: Shanghai Yizhi industrial Limited by Share Ltd Address before: 200434 Hongkou District Memorial Road, Hongkou District, Shanghai, room 1401, room 8 Patentee before: Shanghai Yizhi Enterprise Co., Ltd. |