CN204022709U - The device of the high-purity butanols of a kind of butanols dewatering and recovery - Google Patents
The device of the high-purity butanols of a kind of butanols dewatering and recovery Download PDFInfo
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- CN204022709U CN204022709U CN201320619422.8U CN201320619422U CN204022709U CN 204022709 U CN204022709 U CN 204022709U CN 201320619422 U CN201320619422 U CN 201320619422U CN 204022709 U CN204022709 U CN 204022709U
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Abstract
The utility model relates to the device of the high-purity butanols of a kind of butanols dewatering and recovery, feedstock pump outlet connects preheater shell side entrance, the outlet of preheater shell side connects distillation tower import, base product material divides two-way, one tunnel connects column bottoms pump outlet, one tunnel is connected to reboiler tube side entrance, reboiler tube side outlet line connects base product gas phase entrance, column bottoms pump outlet connects preheater tube side entrance, tower top outlet gas phase connects condenser shell side entrance, condenser shell side outlet phlegma connects moisture decanting vessel entrance, the outlet of decanting vessel oil phase connects reflux pump entrance, reflux pump outlet connects distillation tower top refluxing opening, the outlet of decanting vessel water connects unit for treating water.The mutual heat exchange of high-temp butanol liquid phase of extraction at the bottom of the utility model raw material and tower, has reduced the thermal load of tower bottom reboiler, simultaneously by cooling high-temp butanol at the bottom of tower, is conducive to the storage of the energy-conservation and butanols of device.The butanols purity 99% reclaiming, the rate of recovery of butanols reaches as high as 98.7%.
Description
Technical field
The utility model relates to a kind of device of butanols dewatering and recovery high purity butanols.
Background technology
Butanols is a kind of important Chemicals, serves many purposes, and is used as chemical feedstocks in plastics industry, in food and perfume industry, is used as extraction agent.
Along with the maturation of biofermentation technique in recent years, bioenergy butanols is come into people's the visual field, and it is New-type fuel of new generation, is called as s-generation biofuel.Do not changing under the prerequisite of engine, gasoline can allow to mix mutually with 20% butanols.Carbonatoms in butanol molecules is more than ethanol, and unit volume consumption can discharge more multipotency, has energy density high, the feature that economic and practical is good.And butanols wetting ability than ethanol a little less than, in the time mixing with arbitrary proportion with gasoline, the vapor pressure of generation is low, little to the corrodibility of pipeline, be convenient to pipeline carry.Therefore, butanols is more suitable for widespread use in current international energy situation.
Owing to being subject to the restriction of technology and resource, China's butanols is underproduce to meet the demand of domestic market, and the phenomenon of inadequate supply occurs frequent, all needs a large amount of imports to meet domestic needs every year, therefore, is also being subject in price abroad very large impact.More than 200 ten thousand tons of world's butanols consumptions, 2011 annual requirements are 3,400,000 tons, the five-year consumption average growth rate per annum is expected to be 4%
[1].
Therefore, the technology of exploitation separating-purifying butanols plays an important role to the market of butanols.In the butanols that biological fermentation produces and used solvent butanols, all contain moisture, fourth alcohol and water has azeotropic, and water and butanols have partial miscibility while mixing, and the purity of butanols is difficult to purify.So by the moisture removal in butanols, can obtain the butanols that purity is higher, can improve the value of butanols.Application number is that 201080032088.5 patent is to utilize organic extractant that butanols is extracted at the bottom of tower to then separating-purifying butanols, after this technique dehydration, also needs to separate into row extraction agent again, and technique is more complicated, and reference mark is many.The utility model people can separate butanols by a distillation tower through experimental studies have found that with water, and obtains water and the better stratification temperature scope of oil phase by many experiments, removes moisture, obtains high-purity butanols.
Reference:
[1] Liu Jia, stripping absorption method is extracted the research of acetone-butanol technique, Hebei University of Science and Technology's academic dissertation, 2011.
Summary of the invention
The purpose of this utility model, is to provide a kind of device of butanols dewatering and recovery high purity butanols.
The related device of this technique utility model is simple, and cost is low, safe and reliable, easily operation.The rate of recovery of butanols and purity are all higher.
The utility model reclaims high purity butanols device, equipment connection is as follows: feedstock pump outlet connects preheater shell side entrance, the outlet of preheater shell side connects distillation tower import, base product material divides two-way, one tunnel connects column bottoms pump outlet, one tunnel is connected to reboiler tube side entrance, reboiler tube side outlet line connects base product gas phase entrance, column bottoms pump outlet connects preheater tube side entrance, tower top outlet gas phase connects condenser shell side entrance, condenser shell side outlet phlegma connects moisture decanting vessel entrance, the outlet of decanting vessel oil phase connects reflux pump entrance, reflux pump outlet connects distillation tower top refluxing opening, the outlet of decanting vessel water connects unit for treating water.
Operating process of the present utility model is as follows:
The utility model, for the butanols of moisture and a small amount of impurity, by the moisture removal in butanols, obtains highly purified butanols by equipment such as distillation tower, reboiler, condenser, moisture decanting vessels.Its technique narration: the crude product butanols of moisture content and impurity is through fresh feed pump, controlling stable flow enters after feed preheater is preheating to suitable temp to enter in rectifying tower, or directly enter tower without preheating, the mutual mass transfer of process gas-liquid in tower, the gas phase mixture of overhead extraction fourth alcohol and water, after condensing to optimal temperature, enter moisture decanting vessel, layered buffer passage and observation visor are set in decanting vessel, make moisture and butanols in selected service temperature lower leaf, aqueous phase layer through valve pipe control after water treatment, discharge, oil phase layer delivers in tower, in tower distribute after flow downward with tower in rise steam form countercurrent mass transfer.At the bottom of tower, a liquid phase part adds thermosetting rising steam through reboiler; Another part through column bottoms pump, is controlled stable flow extraction, and at the bottom of tower, the high-temperature liquid-phase of extraction is high product purity butanols, the incoming stock preheater of high-temp butanol give raw material preheating, and butanols is cooled to enter after suitable temperature products pot by raw material and stores and sell.
Described distillation column equipment is vertical Space Facilities, its inner tower inner member of installing; Described moisture decanting vessel is non-pressure vessel, and bottom is water layer phase, and top is butanols oil phase, and internal tank is installed buffering road, and visor is installed in outside below layering place.Described condenser, preheater, reboiler are interchanger.Described equipment can design different size dimensions according to treatment capacity difference.
The utility model device, the mutual heat exchange of high-temp butanol liquid phase of extraction at the bottom of raw material and tower, has reduced the thermal load of tower bottom reboiler, simultaneously by cooling high-temp butanol at the bottom of tower, is conducive to the storage of the energy-conservation and butanols of device.
The utility model device after design and operation, the butanols purity 99% of recovery, the rate of recovery of butanols reaches as high as 98.7%.
Brief description of the drawings
Fig. 1: the high-purity butanols conventional equipment of the utility model butanols dewatering and recovery figure;
Fig. 2: the high-purity butanols of the utility model butanols dewatering and recovery directly utilizes liquid level difference to enter tower apparatus figure;
Wherein: 1, fresh feed pump; 2, feed preheater; 3, distillation tower; 4, reboiler; 5, column bottoms pump; 6, condenser; 7,7, moisture decanting vessel; 8, reflux pump.
Logistics explanation: S1 raw material enters preheater pipeline; S2 preheater by-pass line; After S3 preheating, material enters tower pipeline; S4 materials at bottom of tower enters column bottoms pump pipeline; S5 materials at bottom of tower enters reboiler pipeline; S6 column bottoms pump enters preheater pipeline; S7 reboiler steam is entered tower pipeline; S8 top gaseous phase enters condenser pipeline; S9 phlegma water inlet point decanting vessel pipeline; Reflux pump pipeline is entered in the extraction of S10 oil phase; S11 reflux pump enters tower pipeline; S12 water extraction pipeline.
Embodiment
Below in conjunction with drawings and Examples, this device and technique are described in further detail.
The utility model reclaims the equipment connection of high purity butanols device as Fig. 1, feedstock pump 1 exports S1 pipeline and connects preheater 2 shell side entrances, preheater 2 shell side outlet line S3 connect distillation tower 3 imports, distillation tower 3 substrate material divide two-way, one road S4 connects column bottoms pump 5 and exports, one road S5 is connected to reboiler 4 tube side entrances, reboiler 4 tube side outlet line S7 connect distillation tower 3 spirit phase entrances, column bottoms pump outlet line S6 connects preheater 2 tube side entrances, tower top outlet gas phase pipeline S8 connects condenser 6 shell side entrances, condenser 6 shell side outlet phlegma pipeline S9 connect moisture decanting vessel 7 entrances, decanting vessel 7 oil phase outlet pipe line S10 connect reflux pump 8 entrances,
The utility model is introduced high purity butanols recovery method and device, and wherein main equipment comprises feed preheater 2, distillation tower 3, tower bottom reboiler 4, overhead condenser 6, moisture decanting vessel 7.Technique is as shown in Figure 1: the crude product raw material butanols of moisture content and impurity is through fresh feed pump 1, and by entering feed preheater 2 tube side preheatings after feed rate meter and valve control regime flow, the raw material after preheating is to distillation tower 3 chargings.In material tower, after gas-liquid mass transfer separates, tower top obtains fourth alcohol and water and mixes gas phase, enters the whole condensations of overhead condenser 6 by pipeline.Condensed liquid phase all enters moisture decanting vessel 7, and the temperature that enters decanting vessel by entering the temperature of condenser heat-eliminating medium and flow control makes the layering in decanting vessel of butanols and water mixture, and upper strata is oil phase butanols, and lower floor is water.The extraction of upper oil phase butanols is controlled regime flow by reflux pump 8 and is entered distillation trim the top of column, if mounting height enough can directly utilize liquid level difference to enter in tower, as shown in Figure 2, lower layer of water is entered after water treatment system is processed and discharged by valve control.At the bottom of tower, obtain high-purity liquid phase butanols, butanols by tower at the bottom of a discharging mouth of pipe part enter reboiler 4, after heating by reboiler, form vapour-liquid mixed phase and return in distillation tower, for system provides rising steam; Another part high temperature, by column bottoms pump 5, enters feed preheater after tower bottom flow amount meter and valve control regime flow, and the high-temp butanol after preheater heat exchange is cooled to optimal temperature, can be used as direct distribution or storage.This system operation condition: input of column temperature is 30～85 DEG C; Cooled product butanols temperature is 40～50 DEG C; The temperature of overhead condenser is 71～110 DEG C; The temperature of moisture decanting vessel is 70～110 DEG C; The temperature of distillation tower is 74～112 DEG C, and pressure is 50～202kPa.
Embodiment 1
Utilize the utility model device to carry out pilot scale research, the crude product butanols solvent that raw material is certain factory, it consists of butanols massfraction 85%, quality mark 14%, formaldehyde massfraction 1%.After processing by the utility model method, reclaim butanols, operational condition is: feeding temperature is 85 DEG C; Cooled product butanols temperature is 40 DEG C; After the condensation of overhead condenser, temperature is 90 DEG C; The temperature of moisture decanting vessel is 90 DEG C; The temperature of distillation tower is 101 DEG C, and pressure is 105kPa(absolute pressure); Heating source is 3MPa(absolute pressure) saturated vapor; Circulating water pressure is 3～4MPa(absolute pressure), temperature is 30 DEG C.Technique obtains the results are shown in Table 1.
Table 1 art breading result
Obtained by data in table 1, the purity after the crude product butanols solvent in factory is purified is 98.8%, and calculating butanols yield is 98.65%.
The utility model device, in the time that equipment mounting height is enough, the installation of condenser and decanting vessel can be placed on the place higher than tower top, at this moment reflux pump can, form flow by gravity, as accompanying drawing 2 connects.In the time that mounting height space is inadequate, condenser and decanting vessel installation site, lower than trim the top of column mouth, now need to install reflux pump, form forced refluence, as accompanying drawing 1 connects.
Embodiment 2
The research of the utility model lab scale, preparation raw material component is butanols massfraction 80%, quality mark 20%.Operational condition is that raw material feeding temperature is 30 DEG C; Cooled product butanols temperature is 50 DEG C; After the condensation of overhead condenser, temperature is 90 DEG C; The temperature of moisture decanting vessel is 85 DEG C; The temperature of distillation tower is 92 DEG C, and pressure is 102kPa(absolute pressure); Heating source is electrically heated; Water coolant is that pressure is 3～4MPa(absolute pressure), temperature is 25 DEG C.Small testing device mounting height space is enough, so the installation of condenser and decanting vessel can be placed on the place higher than tower top, trim the top of column adopts flow by gravity form, as accompanying drawing 2.Lab scale research obtains result as following table 2:
Table 2 lab scale result of study
Obtained by data in table 2, the purity after feedstock purification is 99.3%, and calculating butanols yield is 98.0%.
Embodiment 3
The utility model processing simulation, feed composition is butanols massfraction 70%, quality mark 10%.Raw material feeding temperature is 60 DEG C; Cooled product butanols temperature is 43 DEG C; After the condensation of overhead condenser, temperature is 71 DEG C; The temperature of moisture decanting vessel is 70 DEG C; The temperature of distillation tower is 74 DEG C, and pressure is 50kPa(absolute pressure).Lab scale research obtains result as following table 3:
Table 3 lab scale result of study
Obtained by data in table 3, the purity after feedstock purification is 98.2%, and calculating butanols yield is 93.6%.
When simulator equipment is installed, when the installation of condenser and decanting vessel is during higher than tower top, reflux pump can, form flow by gravity, as accompanying drawing 2 connects.When condenser and decanting vessel position are during lower than trim the top of column mouth, reflux pump is installed, form forced refluence, as accompanying drawing 1 connects.
Embodiment 4
The industrialization of the utility model technique expands simulation, and feed composition is butanols massfraction 80%, quality mark 20%.Raw material feeding temperature is 50 DEG C; Cooled product butanols temperature is 47 DEG C; After the condensation of overhead condenser, temperature is 110 DEG C; The temperature of moisture decanting vessel is 110 DEG C; The temperature of distillation tower is 112 DEG C, and pressure is 202kPa(absolute pressure).Simulation obtains result following 4:
Table 3 lab scale result of study
Obtained by data in table 4, the purity after feedstock purification is 99%, and calculating butanols yield is 98.8%.
When industrialization expansion instrument is installed, equipment is higher, considers that overhaul of the equipments is easy for installation, processing ease, and suggestion condenser and decanting vessel are placed on lower, reflux pump forced refluence are installed, as accompanying drawing 1 connects.
From above result, the utility model has proposed effective ways and device for crude product Butanol Recycling problem, and the butanols of market demands more than 98% just can meet industrial requirement.And higher through benzene utility model butanols purity after treatment, can reach more than 99%, yield also can reach more than 98.6.Therefore in the recovery of the proposition of this patent to butanols and device operation, there is important meaning.
Claims (2)
1. the device of a butanols dewatering and recovery high purity butanols, it is characterized in that, feedstock pump outlet connects preheater shell side entrance, the outlet of preheater shell side connects distillation tower import, base product material divides two-way, one tunnel connects column bottoms pump outlet, one tunnel is connected to reboiler tube side entrance, reboiler tube side outlet line connects base product gas phase entrance, column bottoms pump outlet connects preheater tube side entrance, tower top outlet gas phase connects condenser shell side entrance, condenser shell side outlet phlegma connects moisture decanting vessel entrance, the outlet of decanting vessel oil phase connects reflux pump entrance, reflux pump outlet connects distillation tower top refluxing opening, the outlet of decanting vessel water connects unit for treating water.
2. device as claimed in claim 1, is characterized in that described condenser, preheater and reboiler are interchanger.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320619422.8U CN204022709U (en) | 2013-09-30 | 2013-09-30 | The device of the high-purity butanols of a kind of butanols dewatering and recovery |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201320619422.8U CN204022709U (en) | 2013-09-30 | 2013-09-30 | The device of the high-purity butanols of a kind of butanols dewatering and recovery |
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| CN204022709U true CN204022709U (en) | 2014-12-17 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105418423A (en) * | 2015-12-21 | 2016-03-23 | 南京荣欣化工有限公司 | Method and device for benzene-removal and purification of n-propyl acetate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105418423A (en) * | 2015-12-21 | 2016-03-23 | 南京荣欣化工有限公司 | Method and device for benzene-removal and purification of n-propyl acetate |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141217 Termination date: 20190930 |