CN101054368A - Method and apparatus for purification of furfuryl alcohol - Google Patents
Method and apparatus for purification of furfuryl alcohol Download PDFInfo
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- CN101054368A CN101054368A CNA2007101104493A CN200710110449A CN101054368A CN 101054368 A CN101054368 A CN 101054368A CN A2007101104493 A CNA2007101104493 A CN A2007101104493A CN 200710110449 A CN200710110449 A CN 200710110449A CN 101054368 A CN101054368 A CN 101054368A
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Abstract
The present invention fine purification technique of crude product furfuryl alcohol and device thereof, wherein water and light component of crude product furfuryl alcohol is removed in dehydration tower, then completed product of furfuryl alcohol is prepared by distilling in rectifying still, last of all furfuryl alcohol crude product which is deposited inrectifying still and contain deposited matter and high-boiling product is transported to another distilling still to inline process, completed product of furfuryl alcohol is separated out and collected, and the residue is discharged. The present invention is characterized in that said 3 steps process is continuous distillation technique, which resolve the present problem of small distillation output of single unit equipment, low completed product recovery rate, large equipment investment, frequent maintenance and long operation interval act existed in discontinuous way distillation technique used for fine purification of furfuryl alcohol crude product.Use of above rectifying still and distilling still used for processing high-boiling product also resolve the problem, which heating pipe of evaporator is easily scaled in the existent technology.
Description
Technical field
The present invention relates to a kind of process for refining and device thereof of crude product furfuryl alcohol, especially relate to a kind of crude product purification of furfuryl alcohol technology and device thereof when preparing furfuryl alcohol with the furfural shortening.
Background technology
Furfuryl alcohol has another name called furfuralcohol, is the product of furfural shortening.Be mainly used in the raw material in the industry such as the dilution of tackiness agent, anticorrosive coating, synthetic resins of machine-processed foundary industry and properties-correcting agent and synthetic rubber, agricultural chemicals.The production of furfuryl alcohol industrialization already, the processing method that the furfural shortening is produced the crude product furfuryl alcohol all is to adopt quantity-produced technology, yet, still generally adopt step production technique to the distillation of crude product furfuryl alcohol is refining at home at present, promptly in a still kettle, feed intake earlier, after water and light constituent are sloughed in distillation, continue distillation and obtain the finished product furfuryl alcohol, with the residuum discharging, and then feed intake, once more distillation.This step distil process exists single complete equipment distillation amount little, and the finished product rate of recovery is low, and maintenance is frequent, operation room is every defective such as long.France Rhone Poulenc company produces in the technology of furfuryl alcohol at the furfural shortening, purification of furfuryl alcohol adopts " four towers " technology (to see the 2nd phase of " modern chemical industry " nineteen ninety, exercise question is " a furfuryl alcohol progress in Production Technology "), so-called " four towers " is cut light tower, takes off furfural tower, treating tower and take off heavies column, though this technology can be produced purer furfuryl alcohol, but also be step production technique, also exist facility investment big except the above-mentioned shortcoming that has batch process, steam, electric power equal energy source consume high shortcoming.
Summary of the invention
Continuous distillation process and device thereof when for this reason, one of technical problem to be solved by this invention is to propose a kind of crude product purification of furfuryl alcohol.
Two of technical problem to be solved by this invention is to propose the device that a cover can prevent that easy foulant in the crude product purification of furfuryl alcohol process, high boiling material from stopping up the vaporizer bonding.
For solving the problems of the technologies described above, a kind of crude product purification of furfuryl alcohol of the present invention, described process for purification comprises:
A. water and light constituent in the described crude product furfuryl alcohol are sloughed in crude product dehydration;
B. rectifying is distilled the above-mentioned crude product furfuryl alcohol of sloughing water and light constituent, removes the high boiling material that boiling point is higher than furfuryl alcohol, obtains the furfuryl alcohol finished product;
C. high boiling material is handled, and the high boiling material of removing in step b that contains furfuryl alcohol is further distilled, and the furfuryl alcohol finished product that obtains is collected, the residuum discharging;
Wherein, described three steps be continuously rather than intermittent type carry out.
Described three steps are carried out in dehydration tower, rectifying still and still kettle respectively, and between the described step are that the continuous conveying of feed liquid is to realize by the vacuum difference between described three devices continuously.
Described b step and c step be to take out in conjunction with pump again by the vacuum difference to carry the mode of feed liquid to realize continuously.
Described process for purification comprises:
A. keep in the described dehydration tower vacuum tightness be-0.6～-0.8mpa, and control that temperature is 80-125 ℃ in the described dehydration tower, the crude product furfuryl alcohol is sloughed water and light constituent in described dehydration tower, the crude product furfuryl alcohol of sloughing water and light constituent enters described rectifying still from described dehydration tower bottom;
B. the crude product furfuryl alcohol of sloughing water and light constituent in step a is admitted in the described rectifying still because of the vacuum difference between described dehydration tower and the described rectifying still, vacuum tightness in the described rectifying still remains on-0.85～-0.9mpa, temperature is controlled at 100-110 ℃, the furfuryl alcohol finished product that distills out is collected, and throw out, high boiling material etc. sinks in the settler of described rectifying still bottom;
C. take out the mode of feed liquid in conjunction with pump by the vacuum difference, throw out in the described settler, high boiling material be pumped in the described still kettle handle, the vacuum tightness of described still kettle remains on-0.95～-0.98mpa, temperature is controlled at 120-145 ℃, the finished product furfuryl alcohol that distills out is collected, the residuum discharging.
After the every continuous still battery 5-20 of described still kettle hour, described pump is stopped, treating that described still kettle continued distillation after 0.5-3 hour, high boiling material, throw out are discharged, open described pump and continue to pump feed liquid this moment.
The every continuous still battery of described still kettle after 12 hours stops described pump, treats that described still kettle continued distillation after 1 hour, and high boiling material, throw out are discharged, and open described pump and continue to pump feed liquid this moment.
The invention also discloses a kind of crude product purification of furfuryl alcohol device, be used to realize the process for purification of described crude product furfuryl alcohol, described device comprises successively: dehydration tower is used for sloughing the water and the light constituent of described crude product furfuryl alcohol; Rectifying still distills the above-mentioned crude product furfuryl alcohol of sloughing water and light constituent, removes the high boiling material that boiling point is higher than furfuryl alcohol, obtains the furfuryl alcohol finished product; Still kettle is further distilled described high boiling material, and the furfuryl alcohol finished product that obtains is collected, the residuum discharging; Wherein, be communicated with by the sealing-duct that has valve between described dehydration tower, rectifying still and the still kettle.
Described dehydration tower, rectifying still and still kettle are provided with vacuum extractor, and described three device internal pressures are reduced successively.
In the described dehydration tower vacuum tightness be-0.6～-0.8mpa, the interior vacuum tightness of described rectifying still remains on-0.85～-0.9mpa, the vacuum tightness of described still kettle remains on-0.95～-0.98mpa.
Described rectifying still comprises the evaporator room of being located at top and the settler of being located at the bottom, the bottom of described settler is provided with blow-off pipe, described evaporator room inside is provided with one and goes up vaporizer, the described heating tube of going up vaporizer is connected with described evaporator room, described top of going up vaporizer is higher than the bottom of described evaporator room, described going up between vaporizer and the described settler also is provided with a boiling sparger and a following vaporizer, described boiling sparger is connected with the heating tube bottom of described upward vaporizer and the heating tube top of following vaporizer, the heating tube bottom of following vaporizer is communicated with settler, the periphery of vaporizer also is provided with at least one circulation tube on described, and described circulation tube is communicated with the bottom of evaporator room and the top of settler.
Described still kettle comprises the evaporator room of being located at top and the settler of being located at the bottom, also be provided with a vaporizer between described evaporator room and the described settler, the heating tube of described vaporizer and described evaporator room and described settler are interconnected, the bottom of described settler is provided with blow-off pipe, the top of described vaporizer is higher than the bottom of described evaporator room, outer periphery at described vaporizer is equipped with at least one circulation tube, and described circulation tube is communicated with the bottom of evaporator room and the top of settler.
Described boiling sparger is a hollow cylinder, and the described vaporizer of going up is shell and tube heat exchanger with following vaporizer.
The circulation tube of described rectifying still and described still kettle is uniformly distributed in described periphery of going up vaporizer and described vaporizer respectively.
Described dehydration tower is board-like dehydration tower, bubble-plate column or the valve tray column of evaporator with external heating unit.
The tower height of described tray column is between 10-20m.
Described still kettle is a central circulating tube formula still kettle.
Technique scheme of the present invention compared with prior art has the following advantages, (1) realized preparing the continuous refining process of crude product furfuryl alcohol in the furfuryl alcohol technology with the furfural shortening, improved plant efficiency, improve the distillation total amount and the finished product rate of recovery of furfuryl alcohol, be suitable for the industrialized production of furfuryl alcohol; (2) difference at three operations in the crude product purification of furfuryl alcohol process requires to select for use different distillation plants, when sloughing the crude product furfuryl alcohol of water and light constituent in processing, what use is to have last vaporizer, the peripheral circulation tubular type tubulation heating rectifying still of hollow boiling sparger and following vaporizer, and when handling high boiling material, what use is the peripheral circulation still kettle with a shell and tube evaporator, improved distillation efficiency, simultaneously described rectifying still and being used to is handled the use of the still kettle of high boiling material, make that the speed of circulation of feed liquid in still is fast, compare with technology in the past, shortened the time that feed liquid stops in still, reduced the generation of side reaction, improve the productive rate of furfuryl alcohol, guaranteed the quality of furfuryl alcohol; (3) rectifying still of the present invention and being used to is handled the use of the still kettle of high boiling material, also solved in the purification of furfuryl alcohol process easily foulant, the high boiling material blocking problem that in the heating tube of still kettle, bonds, improved the distillation amount of unit time, prolonged the equipment life cycle, ensure rate of heat transfer, reduced steam consumption; (4) new continuously feeding mode, vacuum are taken out material and are combined with the pumping feed liquid, have also improved the distillation efficiency of furfuryl alcohol.
Description of drawings
For the easier quilt of content of the present invention is clearly understood, below according to a particular embodiment of the invention and in conjunction with the accompanying drawings, the present invention is further detailed explanation, wherein
Fig. 1 is the schematic representation of apparatus that is used for the crude product purification of furfuryl alcohol of the present invention;
Fig. 2 is the synoptic diagram of the board-like dehydration tower of the evaporator with external heating unit that is used to slough water and light constituent of the present invention;
Fig. 3 is the synoptic diagram of the rectifying still in the crude product purification of furfuryl alcohol device of the present invention;
Fig. 4 is the synoptic diagram of the still kettle in the crude product purification of furfuryl alcohol device of the present invention;
Fig. 5 is the structural representation of the central circulating tube formula still kettle of another embodiment that is used to handle the crude product furfuryl alcohol that contains high boiling material of the present invention;
Fig. 6 is that the production of the batch distillation technology of crude product furfuryl alcohol continuous distillation process of the present invention and prior art consumes contrast table.
Reference numeral is expressed as among the figure: the board-like dehydration tower of 1-evaporator with external heating unit, the 2-rectifying still, the 3-still kettle, the 101-valve, the 102-vaporizer, the 103-heating tube, the 104-storage compartment, the 105-vapour outlet, the 106-pipeline, the 107-valve, the 201-evaporator room, the 202-settler, the 203-opening for feed, the 204-blow-off pipe, the last vaporizer of 205-, the 206-sparger that seethes with excitement, vaporizer under the 207-, the 208-circulation tube, the 209-valve, the 210-pneumatic outlet, the 211-pump, the 301-evaporator room, the 302-settler, the 303-opening for feed, the 304-vaporizer, the 305-blow-off pipe, the 306-circulation tube, the 307-pneumatic outlet, 4-central circulating tube formula still kettle.
Embodiment
Fig. 1 is the device synoptic diagram that is used for crude product purification of furfuryl alcohol technology of the present invention, comprise dehydration tower 1, rectifying still 2 and be used to handle the still kettle 3 of high boiling material, connect by the sealing-duct that has valve 107,209 between them, wherein, dehydration tower 1 is the board-like dehydration tower 1 of an evaporator with external heating unit, and referring to Fig. 2, it comprises that external being used to heats vaporizer 102 and a tray column that is used to slough water and light constituent of crude product furfuryl alcohol, because of its structure is a prior art, be not described in detail in this.The crude product furfuryl alcohol is sloughed water and light constituent in the board-like dehydration tower 1 of evaporator with external heating unit, rectifying still 2 is used to remove boiling point and is higher than the impurity of furfuryl alcohol and obtains the furfuryl alcohol finished product, and 3 of still kettles are used for the furfuryl alcohol finished product is further handled and obtained to the crude product furfuryl alcohol that contains more high boiling material that rectifying still 2 is discharged.And the A shown in the figure represents to be used for collecting the container of condensed water and light constituent, and B represents to be used for collecting the container of finished product furfuryl alcohol, and C represents to be used for collecting the container of the high boiling material of discharging from still kettle 3, and D then represents to be used for depositing the feed reservoir of crude product furfuryl alcohol.
Introduce the structure and the working process of rectifying still 2 and still kettle 3 below.
Referring to Fig. 3, rectifying still 2 comprises the evaporator room 201 of being located at top and the settler 202 of being located at the bottom, the middle part of evaporator room 201 sidewalls is provided with opening for feed 203, the bottom of settler 202 is provided with blow-off pipe 204, evaporator room 201 inside are provided with one and go up vaporizer 205, the heating tube of last vaporizer 205 is connected with evaporator room 201, and the top of the heating tube of last vaporizer 205 will be higher than the bottom of evaporator room 201, also be provided with a boiling sparger 206 and a following vaporizer 207 between last vaporizer 205 and the settler 202, boiling sparger 206 is connected with the heating tube bottom of last vaporizer 205 and the heating tube top of following vaporizer 207, the heating tube bottom of following vaporizer 207 is communicated with settler 202, at last vaporizer 205, the periphery of boiling sparger 206 and following vaporizer 207 also is provided with many circulation tubes 208, and circulation tube 208 is round last vaporizer 205 in the present embodiment, boiling sparger 206 and following vaporizer 207 are evenly distributed; Circulation tube 208 is communicated with the bottom of evaporator room 201 and the top of settler 202.The sparger 206 that wherein seethes with excitement is hollow cylinder, and the vaporizer in last vaporizer 205 and the following vaporizer 207 is shell and tube heat exchanger.
Referring to Fig. 4, the structure of still kettle 3 comprises: the evaporator room 301 and the settler 302 of being located at the bottom of being located at top, the middle part of evaporator room 301 sidewalls is provided with opening for feed 303, also be provided with a vaporizer 304 between evaporator room 301 and the settler 302, the heating tube of vaporizer 304 and evaporator room 301 and settler 302 are interconnected, the bottom of settler 302 is provided with blow-off pipe 305, the heating tube top of vaporizer 304 is higher than the bottom of evaporator room 301, outer periphery at vaporizer 304 is equipped with many circulation tubes 306, and circulation tube 306 is communicated with the bottom of evaporator room 301 and the top of settler 302.Circulation tube 306 is evenly distributed round vaporizer 304 in the present embodiment; Vaporizer 304 is a shell and tube heat exchanger.
In still kettle 3,, not only improved distillation efficiency, but also solved the difficult problem of easy foulant, high boiling material easy fouling in the heating tube of vaporizer by using circulation tube.Similarly, in rectifying still 2, pass through to adopt circulation tube, especially also adopt up and down vaporizer and the boiling sparger between the two, improved distillation efficiency more, and solved easy foulant, high boiling material easy long-term puzzlement those skilled in the art's of fouling a difficult problem in the heating tube of vaporizer well.The employing of still kettle 3 in the present invention is mainly used in the crude product furfuryl alcohol that contains more high boiling material that rectifying still 2 is discharged and further handles, and has improved the purification efficiency of furfuryl alcohol, has reduced the pollution to environment.
Set forth the above-mentioned advantage of rectifying still 2 of the present invention and still kettle 3 below by introducing the still-process of feed liquid in apparatus of the present invention.
Still referring to Fig. 3, at first feed liquid enters the bottom of evaporator room 201 from opening for feed 203, flow to settler 202 along circulation tube 208, and enter down along with increasing of liquid level in the heating tube of vaporizer 207, feed liquid is subjected to thermal evaporation to enter boiling sparger 206 in the heating tube of following vaporizer 207, in boiling sparger 206 since the tension force effect steam of liquid reallocate, promptly contain the more steam of liquid and in the heating tube of last vaporizer 205 peripheries, enter evaporator room 201, in the heating tube at last vaporizer 205 middle parts, enter evaporator room 201 and contain the few steam of liquid, because it is little to contain the resistance that the few steam of liquid is subjected in the heating tube of last vaporizer 205, therefore distillation speed and efficient have been improved, the steam that enters evaporator room 201 flows out from pneumatic outlet 210, meanwhile, owing to have potential difference between last vaporizer 205 and the circulation tube 208, those enter the easy foulant of evaporator room 201 along with steam, high boiling material just can not recharge in the heating tube of vaporizer 205 again, but along with the feed liquid of opening for feed input follows endless tube 208 inflow settlers 202, wherein, the less part of density flows to down, and vaporizer 207 has entered the circulation distillation once more, and the big easy foulant of density, high boiling material sinks to the bottom of settler 202 and discharges by blow-off pipe 204, because of easy foulant, high boiling material can in time be discharged, and has also improved distillatory speed and efficient.In addition, adopted by last vaporizer 205, the following vaporizer formed of vaporizer 207 and boiling sparger 206, because last vaporizer 205 and following vaporizer 207 promote mutually, accelerate distillation speed, fundamentally solved easy foulant, the high boiling material easy problem of fouling in the heating tube of vaporizer especially in still.
Also have considerable furfuryl alcohol from the feed liquid that contains high boiling material that the bottom blow-down pipe 204 of rectifying still 2 is discharged, recycle for it is further handled, with the purification efficiency that improves furfuryl alcohol and reduce environmental pollution, spy of the present invention has been equipped with still kettle 3.Please refer to shown in Figure 4, the still-process of still kettle 3 that is used for handling high boiling material is as follows: the high boiling material feed liquid enters the bottom of evaporator room 301 from opening for feed 303, flow to settler 302 along circulation tube 306, and enter along with increasing of liquid level in the heating tube of vaporizer 304, feed liquid is subjected to thermal evaporation to enter evaporator room 301 in the heating tube of vaporizer 304 and discharges from pneumatic outlet 307.Simultaneously, the heated liquid boiling back density in the heating tube diminishes, because of with circulation tube 306 in feed liquid formation density difference rise, produce suction force simultaneously, so just formed continuous round-robin continuous still battery, improved distillation speed and efficient.Protrude in the bottom of evaporator room 301 because of the heating tube top of vaporizer 304, those enter the easy foulant of evaporator room 301 along with steam, high boiling material can not recharge in the heating tube of vaporizer 304 again, but along with the feed liquid of opening for feed 303 inputs follows endless tube 306 inflow settlers 302, wherein, the less part of density flows to and has entered the circulation distillation in the heating tube of vaporizer 304 once more, and the big easy foulant of density, high boiling material sinks to the bottom of settler 302 and in time discharges by blow-off pipe 305, reduce easy foulant and in the heating tube of vaporizer, sticked obstruction, also improved distillation speed and efficient.
From above to rectifying still 2 and be used to handle high boiling material still kettle 3 still-process as can be known, the working process of rectifying still 2 and still kettle 3 is basic identical, and its cardinal principle is also identical promptly all to be to prevent that by improving the speed of circulation of feed liquid in still the bonding obstruction in heating tube of easy foulant, high boiling material from also having improved distillation efficiency simultaneously.
Below come method and apparatus of the present invention is further described in detail with a concrete instance:
The crude product furfuryl alcohol is at the board-like dehydration tower 1 of evaporator with external heating unit shown in Figure 1, continuous distillation process in rectifying still 2 and the still kettle 3 is as follows: valve-off 101,107 and 209, in tray column 1, vacuumize, keep in the tower vacuum tightness-0.6～-0.8mpa between, open valve 101, at this moment in the storage compartment 104 of the crude product furfuryl alcohol heating tube 103 that sucked vaporizer 102 from feed reservoir D continuously and tray column 1, after maintaining an equal level with liquid level in the heating tube 103 by liquidometer control storage compartment 104, valve-off 101, feeding steam gives vaporizer 102 heating, and the interior temperature of control tower is between 80-125 ℃, this moment, the furfuryl alcohol crude product in heating tube 103 and storage compartment 104 was subjected to thermal evaporation, because of the tower height h of tray column 1 is 10-20 rice (referring to Fig. 2), so the water that boiling point is lower can separate after refluxing fully with the higher furfuryl alcohol of light constituent and boiling point, the steam of water and light constituent flows out from distillation outlet 105, after condensation, collect in the container A, the furfuryl alcohol crude product that meanwhile is positioned at 104 bottoms, storage compartment is along pipeline 106 heating tube of inflow evaporator 102 again, enter distillation next time, so move in circles, water and light constituent in the crude product furfuryl alcohol of suction just have been removed, after the oversampling chemical examination is qualified, open valve 107 and 101, since the vacuum degree control in the rectifying still 2-0.85～-0.9mpa, temperature is controlled between 100-110 ℃, therefore after opening valve 107, the furfuryl alcohol crude product of sloughing water and light constituent is just sucked evaporator room 201 bottoms of rectifying still 2 continuously, and flow to settler 202 along circulation tube 208 and enter down in the heating tube of vaporizer 207, the furfuryl alcohol crude product is subjected to the laggard sparger 206 of going into to seethe with excitement of thermal evaporation, the last vaporizer 205 of process enters evaporator room 201 and flows out from pneumatic outlet 210 again, after condenser condenses, collect in the container B the collected finished product furfuryl alcohol that is.And those sink to the big high boiling material that contains the crude product furfuryl alcohol of the density of settler 202 bottoms by the vacuum difference again in conjunction with pump 211 pump mode be pumped to vacuum tightness and be-0.95～-0.98mpa, temperature is in 120-145 ℃ the still kettle 3, and flow to settler 302 along circulation tube 306 and enter in the heating tube of vaporizer 304, the crude product furfuryl alcohol is subjected to that thermal evaporation is laggard goes into evaporator room 301 and flow out from pneumatic outlet 307, after the condenser cooling, collect the furfuryl alcohol finished product in container B, those high boiling material then sink to the bottom of settler 302, after feed liquid is handled 12 hours continuously, close pump 211 (valve 209 is opened), continue about 1 hour of distillation again, guarantee that furfuryl alcohol content is lower than below 6% in the discharge, just be discharged to the high boiling material collecting tank C from the high boiling mixture of blow-off pipe 305 with 302 li of settlers, after discharging is clean, open pump 211, import the next batch feed liquid continuously and make it enter the high boiling material treating processes of next round.
It is to be noted, more than be to the description for the treatment of process for the first time in tray column 1, rectifying still 2 and still kettle 3 of crude product furfuryl alcohol, and after crude product furfuryl alcohol refining the finishing first time in described device, all valves 101,107 and 209 always are unlatching, and promptly the treating process of crude product furfuryl alcohol is a successive processes.
In addition, the main order that pump 211 is installed between rectifying still 2 and still kettle 3 be for accelerate feed liquid from settler 202 to still kettle 3 transfer rate, especially when the feed liquid ratio of viscosities in the settler 202 was big, the effect of using described pump 211 was very tangible.Yet even without pump 211 is installed, described feed liquid still can be drawn into by the vacuum difference between rectifying still 2 and the still kettle 3 in the still kettle 3, even that is to say between rectifying still 2 and still kettle 3 pump 211 is not installed, the treating process of described crude product furfuryl alcohol is still carried out continuously.Therefore, the action of pump 211 can't influence the continuous for the treatment of process of the present invention.
In the present embodiment, liquid levels in the evaporator room 201 of rectifying still 2 otherwise be higher than the top of vaporizer 205, liquid level in the evaporator room 301 of still kettle 3 also otherwise be higher than the top of vaporizer 304, its reason is that the furfuryl alcohol of avoiding containing high boiling material recharges into heating tube, guarantee the liquid level in the vaporizer heating tube simultaneously, to guarantee the vaporization efficiency of heating tube to feed liquid.Wherein, described liquid level is all measured by liquidometer.
On the basis of the foregoing description, can also be when the still kettle 3 that is used to handle high boiling material changes central circulating tube formula still kettle 4 (see figure 5)s of prior art into as another embodiment.Certainly, dehydration tower of the present invention can also not adopt tray column and select the dehydration tower of other prior art for use, such as bubble-plate column, valve tray column etc.
In the present invention, the distillation plant difference of selecting for use at the requirement difference of three operations in the crude product purification of furfuryl alcohol process, thereby distillatory efficient and quality have been improved on the whole, as having selected board-like dehydration tower 1 for use for water and the light constituent removed in the crude product furfuryl alcohol, separate better because of it can make water, light constituent with furfuryl alcohol, and use still kettle not reach this separating effect; When the crude product furfuryl alcohol of water and light constituent is sloughed in processing, what select for use is the peripheral circulation tubular type tubulation heating rectifying still 2 with last vaporizer 205, boiling sparger 206 and following vaporizer 207, because of its energy good antiscale property, and furfuryl alcohol fast good separating effect of speed of circulation in this still; When handling high boiling material, what select for use is the peripheral circulation formula still kettle 3 with a vaporizer 304, its speed of circulation is slow slightly than rectifying still, but can give full play to its effect when processing contains the many crude product furfuryl alcohol of high boiling material, reaches required separating effect and does not cause the waste of steam, electric power etc.The present invention takes out the different device of three step process and carries the method for feed liquid to combine by the vacuum difference between each device and with pump, realized the continuous refining process of crude product furfuryl alcohol, improved plant efficiency, the distillation total amount and the finished product rate of recovery of furfuryl alcohol have been improved, be suitable for the industrialized production of furfuryl alcohol, the production of the batch distillation technology of crude product furfuryl alcohol continuous distillation process of the present invention and prior art consumes contrast table and sees Fig. 6, as can be seen from the table, crude product furfuryl alcohol continuous distillation process of the present invention is compared with the batch distillation technology of prior art, reduce to 12 monthly repairs 1 time for 1 time by 3 original monthly repairs, and whenever obtain the water coolant of 1 ton of furfuryl alcohol finished product consumption and half that steam only is equivalent to interrupter method, the furfuryl alcohol productive rate has but improved 3% simultaneously, moon distillation total amount is compared with interrupter method and has also been improved more than 6 times, this shows, crude product furfuryl alcohol continuous distillation process of the present invention has prolonged the equipment life cycle, reduced energy consumption, improved the distillation total amount and the finished product rate of recovery of furfuryl alcohol, compared with traditional interrupter method and have remarkable advantages.
Obviously, the foregoing description only is for example clearly is described, and is not the qualification to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give exhaustive to all embodiments.And conspicuous variation of being extended out thus or change still are among the protection domain of the invention.
Claims (16)
1. crude product purification of furfuryl alcohol method, it is characterized in that: described process for purification comprises:
A. water and light constituent in the described crude product furfuryl alcohol are sloughed in crude product dehydration;
B. rectifying is distilled the above-mentioned crude product furfuryl alcohol of sloughing water and light constituent, removes the high boiling material that boiling point is higher than furfuryl alcohol, obtains the furfuryl alcohol finished product;
C. high boiling material is handled, and the high boiling material of removing in step b that contains furfuryl alcohol is further distilled, and the furfuryl alcohol finished product that obtains is collected, the residuum discharging;
Wherein, described three steps be continuously rather than intermittent type carry out.
2. crude product purification of furfuryl alcohol method according to claim 1, it is characterized in that: described three steps are carried out in dehydration tower, rectifying still and still kettle respectively, and between the described step are that the continuous conveying of feed liquid is to realize by the vacuum difference between described three devices continuously.
3. crude product purification of furfuryl alcohol method according to claim 1 and 2 is characterized in that: described b step and c step be to take out in conjunction with pump again by the vacuum difference to carry the mode of feed liquid to realize continuously.
4. crude product purification of furfuryl alcohol method according to claim 3 is characterized in that described process for purification comprises:
A. keep in the described dehydration tower vacuum tightness be-0.6～-0.8mpa, and control that temperature is 80-125 ℃ in the described dehydration tower, the crude product furfuryl alcohol is sloughed water and light constituent in described dehydration tower, the crude product furfuryl alcohol of sloughing water and light constituent enters described rectifying still from described dehydration tower bottom;
B. the crude product furfuryl alcohol of sloughing water and light constituent in step a is admitted in the described rectifying still because of the vacuum difference between described dehydration tower and the described rectifying still, vacuum tightness in the described rectifying still remains on-0.85～-0.9mpa, temperature is controlled at 100-110 ℃, the furfuryl alcohol finished product that distills out is collected, and throw out, high boiling material etc. sinks in the settler of described rectifying still bottom;
C. take out the mode of feed liquid in conjunction with pump by the vacuum difference, throw out in the described settler, high boiling material be pumped in the described still kettle handle, the vacuum tightness of described still kettle remains on-0.95～-0.98mpa, temperature is controlled at 120-145 ℃, the finished product furfuryl alcohol that distills out is collected, the residuum discharging.
5. crude product purification of furfuryl alcohol method according to claim 4, it is characterized in that: after the every continuous still battery 5-20 of described still kettle hour, described pump is stopped, treating that described still kettle continued distillation after 0.5-3 hour, high boiling material, throw out are discharged, and open described pump and continue to pump feed liquid this moment.
6. crude product purification of furfuryl alcohol method according to claim 5, it is characterized in that: the every continuous still battery of described still kettle after 12 hours stops described pump, treats that described still kettle continued distillation after 1 hour, high boiling material, throw out are discharged, and open described pump and continue to pump feed liquid this moment.
7. a crude product purification of furfuryl alcohol device is used to realize the described crude product purification of furfuryl alcohol of claim 1 to 6 method, and it is characterized in that: described device comprises successively:
Dehydration tower is used for sloughing the water and the light constituent of described crude product furfuryl alcohol;
Rectifying still distills the above-mentioned crude product furfuryl alcohol of sloughing water and light constituent, removes the high boiling material that boiling point is higher than furfuryl alcohol, obtains the furfuryl alcohol finished product;
Still kettle is further distilled described high boiling material, and the furfuryl alcohol finished product that obtains is collected, the residuum discharging;
Wherein, be communicated with by the sealing-duct that has valve between described dehydration tower, rectifying still and the still kettle.
8. crude product purification of furfuryl alcohol device according to claim 7, it is characterized in that: described dehydration tower, rectifying still and still kettle are provided with vacuum extractor, and described three device internal pressures are reduced successively.
9. crude product purification of furfuryl alcohol device according to claim 8, it is characterized in that: in the described dehydration tower vacuum tightness be-0.6～-0.8mpa, vacuum tightness in the described rectifying still remains on-0.85～-0.9mpa, the vacuum tightness of described still kettle remains on-0.95～-0.98mpa.
10. according to claim 7 or 8 described crude product purification of furfuryl alcohol devices, it is characterized in that: described rectifying still comprises the evaporator room of being located at top and the settler of being located at the bottom, the bottom of described settler is provided with blow-off pipe, described evaporator room inside is provided with one and goes up vaporizer, the described heating tube of going up vaporizer is connected with described evaporator room, described top of going up vaporizer is higher than the bottom of described evaporator room, described going up between vaporizer and the described settler also is provided with a boiling sparger and a following vaporizer, described boiling sparger is connected with the heating tube bottom of described upward vaporizer and the heating tube top of following vaporizer, the heating tube bottom of following vaporizer is communicated with settler, the periphery of vaporizer also is provided with at least one circulation tube on described, and described circulation tube is communicated with the bottom of evaporator room and the top of settler.
11. according to claim 7,8 or 10 described crude product purification of furfuryl alcohol devices, it is characterized in that: described still kettle comprises the evaporator room of being located at top and the settler of being located at the bottom, also be provided with a vaporizer between described evaporator room and the described settler, the heating tube of described vaporizer and described evaporator room and described settler are interconnected, the bottom of described settler is provided with blow-off pipe, the top of described vaporizer is higher than the bottom of described evaporator room, outer periphery at described vaporizer is equipped with at least one circulation tube, and described circulation tube is communicated with the bottom of evaporator room and the top of settler.
12. crude product purification of furfuryl alcohol device according to claim 10 is characterized in that: described boiling sparger is a hollow cylinder, the described vaporizer of going up is shell and tube heat exchanger with following vaporizer.
13. the device according to any described crude product purification of furfuryl alcohol method among the claim 10-12 is characterized in that: the circulation tube of described rectifying still and described still kettle is uniformly distributed in described periphery of going up vaporizer and described vaporizer respectively.
14. the device of crude product purification of furfuryl alcohol method according to claim 7 is characterized in that: described dehydration tower is board-like dehydration tower, bubble-plate column or the valve tray column of evaporator with external heating unit.
15. the device of crude product purification of furfuryl alcohol method according to claim 14 is characterized in that: the tower height of described tray column is between 10-20m.
16. according to claim 7,8,9,14 or 15 described crude product purification of furfuryl alcohol devices, it is characterized in that: described still kettle is a central circulating tube formula still kettle.
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| CN101337952B (en) * | 2008-09-01 | 2010-05-12 | 河南宏业化工有限公司 | Method for separating crude furfuryl alcohol by automatic continuous filter pressing and special equipment thereof |
| CN101863863A (en) * | 2010-06-28 | 2010-10-20 | 宏业生化股份有限公司 | Refining method for crude furfuryl alcohol |
| CN101906087A (en) * | 2010-07-23 | 2010-12-08 | 宏业生化股份有限公司 | Process and device for recovering furfuryl alcohol from high-boiling residues generated in furturyl alcohol preparation by furfural hydrogenation |
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| CN101337952B (en) * | 2008-09-01 | 2010-05-12 | 河南宏业化工有限公司 | Method for separating crude furfuryl alcohol by automatic continuous filter pressing and special equipment thereof |
| CN101863863A (en) * | 2010-06-28 | 2010-10-20 | 宏业生化股份有限公司 | Refining method for crude furfuryl alcohol |
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| CN101906087B (en) * | 2010-07-23 | 2012-12-12 | 宏业生化股份有限公司 | Process and device for recovering furfuryl alcohol from high-boiling residues generated in furturyl alcohol preparation by furfural hydrogenation |
| CN102311411A (en) * | 2011-07-07 | 2012-01-11 | 宏业生化股份有限公司 | Method and device for separating coarse furfuryl alcohol from dead catalyst in furfuryl alcohol production |
| CN105602696A (en) * | 2016-02-25 | 2016-05-25 | 郑莉青 | Full-automatic integrated lubricating-oil reclaiming device and lubricating-oil reclaiming method |
| CN105623830A (en) * | 2016-02-25 | 2016-06-01 | 郑莉青 | Integrated lubricating oil regenerating device and method |
| CN108826320A (en) * | 2018-06-26 | 2018-11-16 | 河南禾力能源股份有限公司 | A kind of furfuryl alcohol high-boiling components and Waste water concentrating liquid mixed combustion apparatus |
| CN111646960A (en) * | 2020-05-25 | 2020-09-11 | 安徽金禾实业股份有限公司 | Recovery method of furfuryl alcohol in 2-methyl furan wastewater |
| CN112409304A (en) * | 2020-12-11 | 2021-02-26 | 安徽金禾实业股份有限公司 | Purification method of intermediate in Grignard section of maltol |
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| CN100551920C (en) | 2009-10-21 |
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Denomination of invention: Method and apparatus for purification of furfuryl alcohol Effective date of registration: 20160302 Granted publication date: 20091021 Pledgee: Industrial Commercial Bank of China Ltd Zhangqiu branch Pledgor: Shengquan Group Co., Ltd., Ji'nan City Registration number: 2016990000130 |
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