CN102933271B - Rectification column for preventing thermal-sensitisation and rectification separation process for preventing thermal-sensitisation of natural material - Google Patents
Rectification column for preventing thermal-sensitisation and rectification separation process for preventing thermal-sensitisation of natural material Download PDFInfo
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Abstract
Disclosed are a rectification column for preventing thermal-sensitisation and a rectification separation process for preventing thermal-sensitisation of natural material. The rectification column for preventing thermal-sensitisation comprises a rectification column (2), T-shaped condenser (4) arranged directly on the top of the rectification column (2) and connected with it without conduits, a baffle (12), a column bottom (3) and a falling-film reboiler (5), wherein the circular baffle (12) is disposed in the T-shaped condenser (4), an annular liquid-collecting slot (20) is disposed between the rectification column (2) and the T-shaped condenser (4) for collecting the liquid condensed in the T-shaped condenser (4) and introducing it into a liquid-collecting tank (6) disposed outside the column, the column bottom (3) is connected with the falling-film reboiler (5); by a centrifugal pump (7) to form a high-speed circulating system, the column bottom (3) has a shape of elongated tube, and the falling-film reboiler (5) is of stumpy shell-and-tube. The rectification column for preventing thermal-sensitisation is used in the rectification separation process for preventing thermal-sensitisation of natural material.
Description
Invention field
The present invention relates to a kind of natural materials anti-temperature-sensitive rectifying separating technology and equipment.
Background technology
The spices of natural materials etc. account for critical role in the industries such as chemical industry, food, medicine.Natural perfume material comprises animality spices and vegetal spice, and wherein animality spices comparatively common are Moschus, ambergris etc.; Vegetal spice kind is many, as essential oil, botany bar gum, oleoresin etc.Artificial flavors comprises some alcohols and ester class.At chemical industry, petrochemical industry, pharmacy, in the industry such as food, separator is absolutely necessary.Traditional rectifying separation comprises that intermittently separated (flow process as shown in Figure 2) and continuous separate, from (flow process as shown in Figure 3), intermittently mainly comprise intermittent fractionation tower, heater, condensation reflux unit in separation process.Its basic procedure is: the disposable material that will distill adds and in tower reactor 29, carries out heating evaporation, the gas producing enters into condenser 26 through rectifying column 25 and is condensed into liquid, condensate liquid part backflow rectifying column, get back to tower reactor and continue to add thermal distillation, another part is extraction, be heated to certain hour after the light component in tower reactor material steams completely, the disposable material by tower reactor is emitted, during no longer supplement material.Continuous separation device is than intermittently separator is many feed arrangement 40 and reboiler 35.Continuous separate from basic procedure be: during driving, add tower bottom of rectifying tower to reach certain liquid level raw material to be distilled, start heating, the condensate liquid of tower top gained all refluxes, the infinite reflux stage does not need feed supplement; The condensate liquid part backflow remainder extraction of flowing out from condenser 34 after the infinite reflux stage finishes, and the liquid that enters tower reactor is also wanted part extraction, remainder enters in reboiler 35 and continues heating evaporation, the gas producing enters in rectifying column 33 and flows from bottom to top, now wants continuous charging constant to guarantee the liquid level of material in tower reactor.The flow process of most rectifying separation all belongs to above both of these case.Such requirements of process is carried out long high-temperature heating to material, for above-mentioned these natural materials, most of to thermo-responsive, tend in separated process due to excess Temperature, the long thermosensitive response that occurs of heated time, as polymerization, dehydration, oxidation, decomposition etc., cause the consequences such as coking, carbon deposit, variable color, fragrance be impaired, the quality of product is reduced, also cause the waste of resource simultaneously.
Summary of the invention
The object of the invention is the natural materials for thermal sensitivity, what solve above-mentioned rectifying separator easily causes this defect of temperature-sensitive, proposes a kind of new natural materials anti-temperature-sensitive rectifying separating technology and equipment.When this technology is specially adapted to be separated in heating, easily there is the substance system of thermal sensitivity reaction, can prevent that it is because product that thermosensitive response causes degrades, thereby keep the intrinsic fine quality of target product.
Object of the present invention can be achieved through the following technical solutions:
A kind of anti-temperature-sensitive rectifying column, as shown in Figure 1, it is by rectifying column 2, T-shaped condenser 4, baffle plate 12, tower reactor 3, falling-film reboiler 5 forms, T-shaped condenser 4 is directly placed in rectifying column 2 tops, centre connects without pipeline, distance is almost nil, in T-shaped condenser 4, be provided with a circular baffle plate 12, in T-shaped condenser 4, the liquid of condensation can not directly enter into rectifying column 2, to avoid interior backflow rambunctious, between rectifying column 2 and T-shaped condenser 4, there is an annular collecting tank 20, be used for collecting the liquid of condensation in T-shaped condenser 4, and introduce in the liquid collecting tank 6 outside tower, rectifying column 2 is plate column or packed tower, packed tower preferably, between tower reactor 3 and falling-film reboiler 5, by centrifugal pump 7, be linked to be high-speed circulating system, tower reactor 3 is elongated tubular product, falling-film reboiler 5 is pyknic shell and tube.
Above-mentioned anti-temperature-sensitive rectifying column, described T-shaped condenser 4, and is connected by flange between rectifying column 2, and the refrigerant of T-shaped condenser 4 is entered by pipeline 18, then flows out from pipeline 19.
Above-mentioned anti-temperature-sensitive rectifying column, described collecting tank 20, is arranged on the position of rectifying column 2 top exits, and the limit mouth of collecting tank 20 is the connector with T-shaped condenser 4 higher than rectifying column 2, and and having space between baffle plate 12, the liquid being condensed in T-shaped condenser 4 can only flow in collecting tank 4.
Above-mentioned anti-temperature-sensitive rectifying column, described baffle plate 12, be welded on the top of rectifying column 2 and T-shaped condensing tower 4 interfaces, there is one section of space with rectifying column 2 tops, can allow up steam pass through, the diameter of baffle plate 12 is greater than the inward flange of collecting tank 20 simultaneously, and in T-shaped like this condenser 4, the liquid of condensation will flow in collecting tank 20, and can directly not enter in rectifying column 2.
Above-mentioned anti-temperature-sensitive rectifying column, described tower reactor 3 is elongated tubulose, and volume is traditional tower reactor 1/10 ~ 1/50, and therefore wherein the time of staying of material also correspondingly significantly shortens, and can not be trapped in hot environment for a long time.
Above-mentioned anti-temperature-sensitive rectifying column, described falling film type tubulation reboiler 5, outward appearance is short and stout (ratio of height to diameter is less than 1) cylinder, under the effect of liquid circulation pump at the bottom of tower, fluid each top-down mean residence time in tubulation is very short, is generally 0.1-3 about second.Therefore,, although be the highest place of temperature in whole process, because the time of contact between material and heated wall is extremely short, therefore the generation of thermosensitive response will effectively be avoided herein.The reboiler of traditional rectifying column is contrary, and material, therein by long-time thermophilic digestion, thermosensitive response occurs and be generally difficult to avoid.
Above-mentioned anti-temperature-sensitive rectifying column, described return-flow system is comprised of pipeline 23, liquid collecting tank 6, pipeline 16, centrifugal pump 8 and pipeline 15, liquid collecting tank 6 is used for collecting the liquid flowing out from collecting tank 20, liquid in liquid collecting tank 6, with centrifugal pump 8, a part is sent back in rectifying column 2 and refluxed, a part is plucked out of as product.
The anti-temperature-sensitive rectifying of a natural materials separating technology, as shown in Figure 1, whole technique is continuous, and it adopts above-mentioned anti-temperature-sensitive rectifying column, and concrete steps are as follows:
Step 1. is reduced to action required pressure (the thermally sensitive temperature point that conventionally operating pressure is controlled to the thing that is distillated is following) by vacuum system 22 by whole rectifying column internal pressure, during driving, mixed material is entered into tower reactor 3 from pipeline 1 by rectifying column 2, when reaching certain liquid level, open pump 7, material in tower reactor 3 is squeezed in falling-film reboiler 5 and heated by pipeline 13 and 14, the gas-liquid mixture producing enters into rectifying column 2 by pipeline 11 under the effect of pressure reduction, carries out rectifying;
Step 2. gas enters into T-shaped condenser 4 and is condensed into liquid, due to baffle plate 12, liquid can only be from all side inflow collecting tanks 20 of baffle plate, again in piping 23 enters into liquid collecting tank 6, then through piping 16 and centrifugal pump 8, the liquid in liquid collecting tank 6 is thrown in rectifying column 2, carry out infinite reflux, T-shaped condenser 4 is placed on directly over rectifying column 2, gas enters in the middle of the tank body of condenser 4, because the distance between rectifying column 2 tops and condenser 4 is almost nil, so the gas in rectifying column 2 can be condensed into rapidly liquid, and be cooled to below thermally sensitive temperature, existence due to baffle plate 12, the liquid being condensed can only be from all side inflows of baffle plate 12 to collecting tank 20,
Step 3. is carried out after full tower equilibrium establishment of a period of time when infinite reflux, beginning extraction, open valve 9 and 10, tower top light component distillate is by valve 10 extraction, the interior higher boiling heavy constituent of tower reactor 3 is by valve 9 extraction, by pipeline 1, start charging simultaneously, make the liquid levels in tower reactor 3 remain on normal level, enter into thus the continuous rectification operational phase.
Advantage of the present invention:
1. with traditional rectifying device (Fig. 2, shown in Fig. 3) compare, anti-temperature-sensitive rectifying column (shown in Fig. 1) adopts T-shaped condenser, greatly shortened the distance between rectifying column and condenser, thereby shortened to greatest extent the time of staying of vapour phase between rectifying tower top and condenser, the steam-energy that rises to like this tower top from rectifying column is condensed into rapidly liquid, and is cooled to below thermally sensitive temperature, can effectively prevent the generation of thermosensitive response between tower top and condenser.
2. in anti-temperature-sensitive rectifying column (shown in Fig. 1), between T-shaped condenser pipe and rectifying column, a circular baffle plate and annular collecting tank have been designed, from T-shaped condenser, the liquid of condensing reflux can only flow in collecting tank like this, thereby prevented that condensate liquid from directly entering in rectifying column, be convenient to accurately control refluxing.
3. with traditional rectifying device (Fig. 2, shown in Fig. 3) compare, anti-temperature-sensitive rectifying column (shown in Fig. 1) has adopted elongated tubular product tower reactor, its volume reduces greatly, it is only 1/50 ~ 1/10 of traditional tower reactor, due to the effect of circulating pump at the bottom of tower, the mean residence time that makes material in tower reactor is only also 1/50 ~ 1/10 of traditional tower reactor again.Like this, just avoided tower reactor material at tower reactor high-temperature area by high cooking, thereby greatly suppressed the generation of thermosensitive response in tower reactor.
4. anti-temperature-sensitive rectifying column (shown in Fig. 1) has adopted the falling film type tubulation reboiler of short and thick structure, compare with the common shell and tube reboiler 35 in traditional rectifying device, the top-down liquid of falling film type tubulation reboiler can be constantly updated gasifying surface, make surface heat transfer respond well, vaporization rate is fast, the time of contact of while liquid and high temperature tubulation inner surface is extremely short, can effectively avoid liquid phase material by overheated and long-time high-temperature heating, has also just effectively avoided the generation of thermosensitive response in heat exchanger.
Accompanying drawing explanation
Fig. 1 is anti-temperature-sensitive rectifying separating technology of the present invention and equipment, and wherein 1 is charging aperture, and 2 is rectifying column, 3 is tower reactor, and 4 is T-shaped condenser, and 5 is falling-film reboiler, 6 is liquid collecting tank, and 7,8 is centrifugal pump, and 9,10,21,24 is valve, 11,13,14 is tower reactor material conveying pipe, and 12 is baffle plate, and 15,16,23 is overhead condensation liquid conveyance conduit, 17 is overhead condensation liquid extraction mouth, 18,19 is cooling medium conveyance conduit, and 20 is collecting tank, and 22 is vacuum system.
Fig. 2 is traditional batch rectifying device, and wherein 25 is rectifying column, and 26 is condenser, and 27 is vacuum system, and 28,30,31 is valve, and 29 is tower reactor.
Fig. 3 is traditional continuous rectification equipment, and wherein 32 is tower reactor, and 33 is rectifying column, and 34 is condenser, and 35 is reboiler, and 36 is vacuum system, and 37,38,39 is valve, and 40 is charging aperture.
Fig. 4 is anti-temperature-sensitive two tower rectifying separating technologies and equipment (embodiment 2 and 3 equipment drawing), and 2 is rectifying column A, and T2 is rectifying column B.
The specific embodiment
Embodiment 1
The thick oil of folium eucalypti and the mixed solution of ethanol are entered to tower reactor 3 by pipeline 1 through rectifying column 2, and rectifying column 2 diameters are 0.15m, and theoretical cam curve is 40, and the total measurement (volume) of tower reactor 3 is 50L, and the ratio of height to diameter of tower reactor is 3:1.Open vacuum system 22, the pressure of whole distillation system is dropped to 400 millimetress of mercury, falling-film reboiler 5 starts heating, and the volume of falling-film reboiler 5 is 500L, and the heat medium temperature of falling-film reboiler 5 is 140 ℃.Open pump 7 simultaneously, make the liquid material circulation in tower reactor 3, the circular flow of centrifugal pump is 40m
3/ h, the vapour phase producing in falling-film reboiler 5 enters rectifying column 2 bottoms together with the feed liquid not being vaporized, vapour phase is through rectifying column 2 separation, and the vapour phase that arrives top is condensed into rapidly liquid and flows into after collecting tank 20 in T-shaped condenser 4, then enters liquid collecting tank 6 by pipeline.Adopt centrifugal pump 8 that condensate liquid in liquid collecting tank is directly squeezed into and in rectifying column 2, carried out total reflux operation.When infinite reflux, carry out after full tower equilibrium establishment of a period of time, beginning extraction, opens valve 9 and 10, reflux ratio is 2/5, by pipeline 1, start the mixed solution with ethanol into the thick oil of folium eucalypti simultaneously, guarantee that in tower reactor 3, liquid levels keeps constant, enter into the continuous rectification stage.In the tower reactor liquid material gathering out 1,8-cineole purity is 99.7%, produced quantity is 300kg/h, compare with conventional continuous still, the time of staying of material in tower reactor significantly shortens, being only 1/40 ~ 1/30 of conventional continuous still, is 1/200 ~ 1/100 of conventional batch distillation, almost can avoid the generation of thermosensitive response completely.Due to this, the rate of recovery of 1,8-cineole certified products can than conventional continuous still, improve more than 3%, and product odour be pure up to more than 98.5%, as clear as crystal.
Embodiment 2
Adopt the separated Turpentine Oil From Pinus Massoniana of two tower flow processs.Similar (as shown in Figure 4) of concrete device structure and method of operating and embodiment 1.Turpentine Oil From Pinus Massoniana is added to distillation system rectifying column A2.Rectifying column A2 diameter is 0.15m, and theoretical cam curve is 40, and the total measurement (volume) of tower reactor 3 is 50L, and the ratio of height to diameter of tower reactor is 3:1.The pressure of rectifying column A2 is controlled the operation for 40mmHg, and the heating-up temperature of falling-film reboiler 5 is 140 ℃.The circular flow of centrifugal pump is 30m
3/ h.Infinite reflux a period of time, rectifying column A1 top temperature control was 90 ℃ of left and right, at top extraction australene after full tower temperature stabilization, produced quantity is 180kg/h, more than its purity 98 %, the yield of australene can reach more than 99.5%, than conventional continuous still, improves more than 8 percentage points.The material of rectifying column A2 still bottom is squeezed into rectifying column BT2 by column bottoms pump 7 and is carried out separation.The pressure of rectifying column BT2 is controlled the operation for 40mmHg, and the heating-up temperature of falling-film reboiler is 150 ℃.The circular flow of centrifugal pump is 30m
3/ h.Its top extraction nopinene, produced quantity is 80kg/h, the terebinthine heavy constituent of bottom extraction, is commonly called as heavy oil.The purity of nopinene is more than 98.5, and yield can reach more than 99.0%, than conventional continuous still, improves more than 7 percentage points.
Compare with conventional continuous still, the time of staying of material in two tower reactors shortens dramatically, and is only 1/60 ~ 1/50 of conventional two tower continuous stills, is 1/500 ~ 1/400 of conventional batch distillation, almost can avoid the thermosensitive response of turpentine oil component completely.
Embodiment 3
Similar with the mode of operation of embodiment 2, dihydromyrcenol, dihydromyrcene, isopropyl alcohol mixture are added to distillation system, by vacuum system, control rectifying column A2 operating pressure 20 millimetress of mercury (the diameter 0.15m of rectifying column A, theoretical cam curve 40), the heating-up temperature of falling-film reboiler 5 is 140 ℃, and the circular flow of centrifugal pump 7 is 40m
3/ h, infinite reflux a period of time after full tower temperature stabilization at rectifying column A2 bottom extraction dihydromyrcenol (produced quantity 300kg/h, reflux ratio 2/5), its its purity to 95.6% of content.Sent into again rectifying column BT2 and carried out rectifying, from rectifying column BT2 top, can be obtained more than 99.5% dihydromyrcenol product.By this anti-heat-sensing device and technological operation, the mean residence time of material in two tower reactors is only 1/50 left and right of conventional two tower continuous stills, is 1/400 left and right of conventional batch distillation.Therefore the yield of dihydromyrcenol can improve 14 percentage points of left and right than conventional continuous still up to more than 92%, and improves more than 20% than conventional batch distillation.Products obtained therefrom smell is pure, without any being charred peculiar smell.
Claims (10)
1. an anti-temperature-sensitive rectifying column, it is characterized in that: it is by rectifying column (2), T-shaped condenser (4), baffle plate (12), tower reactor (3), falling-film reboiler (5) and return-flow system form, T-shaped condenser (4) is directly placed in rectifying column (2) top, centre connects without pipeline, in T-shaped condenser (4), be provided with a circular baffle plate (12), in T-shaped condenser (4), the liquid of condensation can not directly enter into rectifying column (2), between rectifying column (2) and T-shaped condenser (4), there is an annular collecting tank (20), be used for collecting the liquid of condensation in T-shaped condenser (4), and introduce in the liquid collecting tank (6) outside tower, between tower reactor (3) and falling-film reboiler (5), by centrifugal pump (7), be linked to be high-speed circulating system, tower reactor (3) is elongated tubular product, falling-film reboiler (5) is thick and short type shell and tube.
2. anti-temperature-sensitive rectifying column according to claim 1, is characterized in that: described rectifying column (2) is plate column or packed tower.
3. anti-temperature-sensitive rectifying column according to claim 2, is characterized in that: described rectifying column (2) is packed tower.
4. anti-temperature-sensitive rectifying column according to claim 1, is characterized in that: between described T-shaped condenser (4) and rectifying column (2), by flange, be connected, the refrigerant of T-shaped condenser (4) is entered by pipeline (18), then flows out from pipeline (19).
5. anti-temperature-sensitive rectifying column according to claim 1, it is characterized in that: described collecting tank (20), be arranged on the position of rectifying column (2) top exit, the limit mouth of collecting tank (20) is the connector with T-shaped condenser (4) higher than rectifying column (2), and and having space between baffle plate (12), the liquid being condensed in T-shaped condenser (4) can only flow in collecting tank (4).
6. anti-temperature-sensitive rectifying column according to claim 1, it is characterized in that: described baffle plate (12), be welded on the top of rectifying column (2) and T-shaped condensing tower (4) interface, there is one section of space with rectifying column (2) top, can allow up steam pass through, the diameter of baffle plate (12) is greater than the inward flange of collecting tank (20) simultaneously, and in T-shaped condenser (4), the liquid of condensation can only flow in collecting tank (20), and can directly not enter in rectifying column (2).
7. anti-temperature-sensitive rectifying column according to claim 1, is characterized in that: described tower reactor (3) is elongated tubulose.
8. anti-temperature-sensitive rectifying column according to claim 1, it is characterized in that: described falling film type tubulation reboiler (5) outward appearance is short and stout cylinder, under the effect of liquid circulation pump at the bottom of tower, fluid each top-down mean residence time in tubulation is generally 0.1-3 about second.
9. anti-temperature-sensitive rectifying column according to claim 1, it is characterized in that: described return-flow system is comprised of T-shaped condenser condenses liquid efferent duct (23), liquid collecting tank (6), liquid collecting tank efferent duct (16), centrifugal pump (8) and centrifugal pump efferent duct (15), liquid collecting tank (6) is used for collecting the liquid flowing out from collecting tank (20), liquid in liquid collecting tank (6), with centrifugal pump (8), a part is sent back in rectifying column (2) and refluxed, a part is plucked out of as product.
10. adopt the anti-temperature-sensitive rectifying of a natural materials separating technology for anti-temperature-sensitive rectifying column claimed in claim 1, whole technique is continuous, and it adopts anti-temperature-sensitive rectifying column claimed in claim 1, it is characterized in that concrete steps are as follows:
Step 1. is reduced to action required pressure by vacuum system (22) by whole rectifying column internal pressure, during driving, mixed material is entered into tower reactor (3) from pipeline (1) by rectifying column (2), when reaching certain liquid level, open pump (7), material in tower reactor (3) is squeezed in falling-film reboiler (5) and heated by pipeline (13 and 14), and the gas-liquid mixture of generation enters into rectifying column (2) by pipeline (11) under the effect of pressure reduction, carries out rectifying;
Step 2. gas enters into T-shaped condenser (4) and is condensed into liquid, due to baffle plate (12), liquid can only be from all side inflow collecting tanks of baffle plate (12) (20), again in piping (23) enters into liquid collecting tank (6), then through piping (16) and centrifugal pump (8), the liquid in liquid collecting tank (6) is thrown in rectifying column (2), carry out infinite reflux, T-shaped condenser (4) is placed on directly over rectifying column (2), gas enters in the middle of the tank body of condenser (4), because the distance between rectifying column (2) top and condenser (4) is almost nil, so the gas in rectifying column (2) can be condensed into rapidly liquid, and be cooled to below thermally sensitive temperature, existence due to baffle plate (12), the liquid being condensed can only be from all side inflows of baffle plate (12) to collecting tank (20),
Step 3. is carried out after full tower equilibrium establishment of a period of time when infinite reflux, beginning extraction, open valve (9) and valve (10), tower top light component distillate is by valve (10) extraction, the interior higher boiling heavy constituent of tower reactor (3) is by valve (9) extraction, by pipeline (1), start charging simultaneously, make the liquid levels in tower reactor (3) remain on normal level, enter into thus the continuous rectification operational phase.
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| PCT/CN2011/071750 WO2012048550A1 (en) | 2010-10-14 | 2011-03-14 | Rectification column for preventing thermal-sensitisation and rectification separation process for preventing thermal-sensitisation of natural material |
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| CN110141884A (en) * | 2019-05-27 | 2019-08-20 | 中冶焦耐(大连)工程技术有限公司 | The method and system of tower top regurgitant volume are controlled in tar production, benzene hydrogenation process |
| CN113563188A (en) * | 2021-08-06 | 2021-10-29 | 联泓新材料科技股份有限公司 | Method for recovering vinyl acetate from vinyl acetate waste liquid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1555902A (en) * | 2003-12-31 | 2004-12-22 | 天津大学 | Thermosensitive material intermittent rectifying process having side material output and tower kettle cold material storage |
| CN101391152A (en) * | 2008-10-22 | 2009-03-25 | 天津大学 | Double-reboiler batch extraction rectification device and method using absorption heat pump |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1555902A (en) * | 2003-12-31 | 2004-12-22 | 天津大学 | Thermosensitive material intermittent rectifying process having side material output and tower kettle cold material storage |
| CN101391152A (en) * | 2008-10-22 | 2009-03-25 | 天津大学 | Double-reboiler batch extraction rectification device and method using absorption heat pump |
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