CN101265245B - Continuous distillation method and device for refining furfuryl alcohol - Google Patents
Continuous distillation method and device for refining furfuryl alcohol Download PDFInfo
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- CN101265245B CN101265245B CN2008100528411A CN200810052841A CN101265245B CN 101265245 B CN101265245 B CN 101265245B CN 2008100528411 A CN2008100528411 A CN 2008100528411A CN 200810052841 A CN200810052841 A CN 200810052841A CN 101265245 B CN101265245 B CN 101265245B
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- furfuryl alcohol
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- component removing
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Abstract
The invention relates to a continuous rectifying method and a device for refining furfuryl alcohol. The method includes removing heavy components with the boiling point higher than that of furfuryl alcohol in a heavy component removing tower through rectifying, and removing light components with the boiling point lower than that of furfuryl alcohol in a light component removing tower through rectifying. The device comprises the heavy component removing tower 2 and light component removing tower 10 connected through a heavy component removing tower circulating pump 3, a valve and a sealing pipe, wherein a raw material inlet 1 is disposed on the heavy component removing tower 2, the heavy component removing tower and the light component removing tower are respectively provided with the circulating pump 3, a heat exchanger 9, a circulating pump 11 and a heat exchanger 15 at the top thereof, and provided with a reboiler 4 and a reboiler 12 at the bottom thereof, and a product outlet is arranged on the light component removing tower 10. The method really realizes continuous production process of furfuryl alcohol coarse product refining in the furfuryl alcohol manufacture by catalytic hydrogenation of furfural, increases equipment processing capacity and product yield, and reduces energy consumption of coarse product refining, and has the advantages of saved investment, low energy consumption and simple and rapid process route.
Description
Technical field
The present invention relates to the distillation technology field, particularly relate to the continuous distillation method and the device of purification of furfuryl alcohol.
Background technology
Furfuryl alcohol is a kind of important Organic Chemicals, and its purposes is very extensive.Be mainly used in resin, cold resistant plasticizer, fiber, rubber and the medicine etc. of synthetic various functions; Also can be used as solvent, rocket fuel etc.Furfuryl alcohol mainly obtains by the furfural shortening, the production of furfuryl alcohol industrialization already, and the processing method that the furfural shortening is produced the crude product furfuryl alcohol all is a continuous production processes, yet at home the distillation of crude product furfuryl alcohol is made with extra care at present and still generally adopt step production technique, promptly in a still kettle, feed intake earlier, after light constituent is sloughed in distillation, continue distillation and obtain the finished product furfuryl alcohol, residuum is left concentratedly, and then feed intake, redistillation, whole still-process does not have backflow, in fact is simple one-level still-process.There are problems such as single complete equipment treatment capacity is little, product yield is low, facility investment is big, energy consumption is high, labor strength is big in this step distil process.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 there is the high shortcoming of energy consumption in the continuous production of being unrealized except the above-mentioned shortcoming that has batch process.The patent CN101054368A " purification of furfuryl alcohol method and device thereof " of Jinan holy well limited-liability company application has proposed to adopt crude product dehydration, rectifying and high boiling material to handle the continuous processing flow process and the device in three steps, though claim to be successive in this application Patent right requirement, shown that by claim 5 and 6 this technology is semi-continuous.
Summary of the invention
For this reason, technical problem to be solved by this invention is to propose a kind of continuous distillation method and device of purification of furfuryl alcohol.Concrete continuous distillation method and equipment are as follows:
The continuous distillation method of purification of furfuryl alcohol comprises the steps:
A, remove the heavy constituent that boiling point is higher than furfuryl alcohol at weight-removing column by distillation operation;
B, remove the light constituent that boiling point is lower than furfuryl alcohol at lightness-removing column by distillation operation.
The continuous rectificating technique of described purification of furfuryl alcohol is characterized in that described method is:
Weight-removing column internal pressure 10～30kPa, temperature is 107-113.8 ℃, the crude product furfuryl alcohol that removes after the heavy constituent enters lightness-removing column from the weight-removing column cat head; Lightness-removing column internal pressure 10～30kPa, temperature is 103-110.2 ℃, the furfuryl alcohol finished product that removes behind the light constituent is collected; Weight-removing column and lightness-removing column cat head are provided with pump respectively and follow cooling, no gas phase condenser.
Implement the device of the continuous distillation method of purification of furfuryl alcohol, comprise weight-removing column, lightness-removing column, be connected with sealing-duct by weight-removing column recycle pump 3, valve between weight-removing column 2 and the lightness-removing column 10; Wherein raw material 1 inlet is arranged on the weight-removing column 2, and weight-removing column 2 and lightness-removing column 10 are provided with recycle pump 3, interchanger 9, recycle pump 11 and interchanger 15 at cat head respectively, and weight-removing column 2 and lightness-removing column 10 are provided with reboiler 4 and reboiler 12 respectively at the bottom of tower; Lightness-removing column 10 is provided with products export.
Described weight-removing column and lightness-removing column all are packing towers, and reboiler adopts steam or heat-conducting oil heating.
Described weight-removing column and lightness-removing column cat head are provided with pump and follow heat sink; Pump follows heat sink and is made up of recycle pump and interchanger., send back to after interchanger cools on first theoretical stage of cat head liquid phase material extraction on weight-removing column or lightness-removing column cat head second or the 3rd theoretical stage with recycle pump, being connected by sealing-duct between recycle pump, interchanger and the tower connects.
Weight-removing column of the present invention and lightness-removing column cat head all are provided with pump and follow heat sink.Described weight-removing column and lightness-removing column number of theoretical plate are 20-30.Described weight-removing column and lightness-removing column all adopt structured packing and many rounds sparger.
Technique scheme of the present invention compared with prior art has the following advantages: (1) has really realized the continuous production processes with crude product purification of furfuryl alcohol in the furfural shortening system furfuryl alcohol technology, improve device processes ability and product yield, reduced the energy consumption of crude product purification of furfuryl alcohol; (2) select for use the band pump to follow the vacuum rectifying apparatus of heat sink at the continuous rectificating technique of crude product purification of furfuryl alcohol, can reduce full tower pressure drop, prevent that Yin Wendu is too high and cause the material coking, occluding device is for the equipment long-term operation is given security; (3) in industrial application, have advantages such as reduced investment, energy consumption is low, operational path is simple and direct.
Description of drawings
Fig. 1: the continuous distillation method of purification of furfuryl alcohol and device synoptic diagram.
Wherein: 1 crude product furfuryl alcohol; 2 weight-removing columns; 3 weight-removing column recycle pumps; 4 weight-removing column reboilers; 5 weight-removing column extraction pumps; 6 heavy constituent; 7 heating mediums go out; 8 heating mediums are gone into; 9 weight-removing column interchanger; 10 lightness-removing columns; 11 lightness-removing column recycle pumps; 12 lightness-removing column reboilers; 13 lightness-removing column extraction pumps; 14 furfuryl alcohol products; 15 weight-removing column interchanger; 16 light constituents; 17 vacuum systems
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail, but the present invention is not limited to this.
Accompanying drawing is that the present invention is used for crude product purification of furfuryl alcohol continuous rectificating technique schematic flow sheet, comprises weight-removing column 2 and lightness-removing column 10, is communicated with by weight-removing column recycle pump 3, valve and sealing-duct between them.Wherein weight-removing column and lightness-removing column all are packing towers, adopt structured packing and many rounds sparger.Crude product furfuryl alcohol 1 is sent into weight-removing column 2 through feedstock pump by head tank and is carried out the continuous rectification operation, removes heavy constituent 6.Control by vacuum system 17 keeps working pressure 10～30kPa (absolute pressure) in the weight-removing column 2, by the heating medium (steam or thermal oil) that adjust to feed weight-removing column reboiler 4 go into 8 and heating medium (steam or thermal oil) go out 7 amount and control and add heat, and then service temperature is 107～113.8 ℃ in the maintenance tower.Pump is set follows cooling for reducing full tower pressure drop weight-removing column 2 cats head, weight-removing column recycle pump 3 is with liquid phase material extraction from second or the 3rd theoretical stage of weight-removing column 2, part cools through interchanger 9 and sends back to 60 ℃ on first theoretical stage of weight-removing column 2, residue does not enter interchanger partially liq material and directly sends on the tenth theoretical stage of lightness-removing column 10 by sealing-duct, and the furfuryl alcohol crude product concentration that removes heavy constituent reaches 96% (wt).The heavy constituent 6 of weight-removing column 2 tower stills are by extraction pump 5 extraction and send system in the tower.Control by vacuum system 17 keeps keeping in the lightness-removing column 10 working pressure 10～30kPa (absolute pressure), by the heating medium (steam or thermal oil) that adjust to feed lightness-removing column reboiler 12 go into 8 and heating medium (steam or thermal oil) go out 7 amount and control and add heat, and then keep in the tower 97.5～110.2 ℃ of service temperatures.For reducing full tower pressure drop, lightness-removing column 10 also is provided with pump at cat head and follows cooling, lightness-removing column recycle pump 11 is with the second or three piece theoretical stage extraction of liquid phase material from lightness-removing column 10, after sending into interchanger 15 through sealing-duct and cooling to 60 ℃, part is sent back on first theoretical stage of lightness-removing column 10, and the remainder liquid material is light constituent 16 extraction.Remove the product that contains furfuryl alcohol 98.5% (wt) behind the light constituent and send into the product jar through lightness-removing column extraction pump 13 as furfuryl alcohol product 14 from lightness-removing column tower still.Because of this crude product purification of furfuryl alcohol continuous rectificating technique flow process and device thereof are at the continuous operation state, and control weight-removing column and lightness-removing column internal pressure, and then guarantee that tower still temperature can be not too high, can prevent coking and blocking.Crude product purification of furfuryl alcohol continuous rectificating technique flow process of the present invention and device thereof compared with prior art can be realized furfuryl alcohol quality 98.5% (wt) that reach international standards, and yield reaches 97%, 0.64 ton of/ton furfuryl alcohol of steam consumption, 29 tons of/ton furfuryl alcohols of cooling-water consumption.From above-mentioned data as seen, the semi-batch technology of the patent CN101054368A " purification of furfuryl alcohol method and device thereof " of the batch distillation technology of crude product purification of furfuryl alcohol continuous rectificating technique flow process of the present invention and prior art and Jinan holy well limited-liability company application is compared, running period was by original 3 months, 12 monthly repairs extend to 36 monthly repairs successively successively, and whenever obtain 1 ton of purity is that the water coolant of 98.5% furfuryl alcohol product consumption is reduced to 29 tons by original 81.5 tons and 42.2 tons, steam consumption is by original 1.2 tons, 0.75 ton drops to 0.64 ton, this shows, crude product purification of furfuryl alcohol continuous rectificating technique flow process of the present invention and apparatus and process flow process thereof are simple, facility investment is few, prolonged the equipment operation cycle, reduced energy consumption, improved the yield of furfuryl alcohol, compared with patent CN101054368A " purification of furfuryl alcohol method and device thereof " the semi-batch technology of traditional batch distillation technology and Jinan holy well limited-liability company application and have significant advantage.
Wherein subordinate list is the production consumption contrast of the patent CN101054368A " purification of furfuryl alcohol method and device thereof " of crude product purification of furfuryl alcohol continuous rectificating technique flow process of the present invention and prior art and the application of Jinan holy well limited-liability company.
| Distil process | Moon distillation total amount (T/5m 3Still) | Furfuryl alcohol yield (%) | Steam (T/T furfuryl alcohol) | Water coolant (T/T furfuryl alcohol) | Running period (moon) |
| Batch technology | 220 | 94 | 1.2 | 81.5 | 3 |
| Semi-batch technology | 1350 | 97 | 0.75 | 42.2 | 12 |
| Continuous processing | 7347 | 97 | 0.64 | 29.0 | 36 |
The continuous distillation method and the device of the purification of furfuryl alcohol that the present invention proposes, be described by embodiment, person skilled obviously can be in not breaking away from content of the present invention, spirit and scope to making method as herein described with device is changed or suitably change and combination, realize the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (4)
1. the continuous distillation method of purification of furfuryl alcohol is characterized in that:
A, remove the heavy constituent that boiling point is higher than furfuryl alcohol at weight-removing column by distillation operation;
B, remove the light constituent that boiling point is lower than furfuryl alcohol at lightness-removing column by distillation operation;
Weight-removing column internal pressure 10～30kPa, temperature is 107113.8 ℃, the crude product furfuryl alcohol that removes after the heavy constituent enters lightness-removing column from the weight-removing column cat head; Lightness-removing column internal pressure 10～30kPa, temperature is 103-110.2 ℃.
2. implement the device of the method for claim 1, comprise weight-removing column, lightness-removing column, be connected with sealing-duct by weight-removing column recycle pump (3), valve between weight-removing column (2) and the lightness-removing column (10); It is characterized in that raw material (1) inlet is arranged on the weight-removing column (2), weight-removing column (2) cat head is provided with recycle pump (3), interchanger (9); Lightness-removing column (10) cat head is provided with recycle pump (11) and interchanger (15); Be provided with reboiler (4) at the bottom of weight-removing column (2) tower, be provided with reboiler (12) at the bottom of lightness-removing column (10) tower; Lightness-removing column (10) is provided with products export.
3. device as claimed in claim 2 is characterized in that described weight-removing column and lightness-removing column all are packing towers, and reboiler adopts steam or heat-conducting oil heating.
4. device as claimed in claim 3, it is characterized in that described recycle pump is with liquid phase material extraction on weight-removing column or lightness-removing column cat head second or the 3rd theoretical stage, send cat head after interchanger cools back to, being connected by sealing-duct between recycle pump, interchanger and the tower connects.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100528411A CN101265245B (en) | 2008-04-22 | 2008-04-22 | Continuous distillation method and device for refining furfuryl alcohol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100528411A CN101265245B (en) | 2008-04-22 | 2008-04-22 | Continuous distillation method and device for refining furfuryl alcohol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101265245A CN101265245A (en) | 2008-09-17 |
| CN101265245B true CN101265245B (en) | 2011-07-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2008100528411A Expired - Fee Related CN101265245B (en) | 2008-04-22 | 2008-04-22 | Continuous distillation method and device for refining furfuryl alcohol |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107141274A (en) * | 2017-06-21 | 2017-09-08 | 山东诺生物质材料有限公司 | A kind of extraction process of the methylfuran of furfuryl alcohol accessory substance 2 |
| CN109796484B (en) * | 2019-02-02 | 2020-04-07 | 苏州金宏气体股份有限公司 | Method and system for breaking azeotropic distillation of tetraethoxysilane |
| 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 |
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Granted publication date: 20110720 Termination date: 20210422 |