CN207944039U - A kind of reclamation set of fusel oil and the process units of ammonia from coal - Google Patents
A kind of reclamation set of fusel oil and the process units of ammonia from coal Download PDFInfo
- Publication number
- CN207944039U CN207944039U CN201721184780.5U CN201721184780U CN207944039U CN 207944039 U CN207944039 U CN 207944039U CN 201721184780 U CN201721184780 U CN 201721184780U CN 207944039 U CN207944039 U CN 207944039U
- Authority
- CN
- China
- Prior art keywords
- fusel oil
- methanol
- tower
- concentration tower
- steam
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The utility model is related to a kind of reclamation set of fusel oil and the process units of ammonia from coal, belong to Pervaporation Technology field.Including：Concentration tower, for carrying out concentrate to fusel oil；Segregator is connected at the top of concentration tower, for flowing back after the overhead vapor partial condensation to concentration tower；Heating device is connect with the gaseous phase outlet of segregator, for being heated to steam；Pervaporation membrane separator is connected to heating device, for being dehydrated to steam；Treating column is connected to Pervaporation membrane separator, and the distillation for carrying out methanol to dewatered steam is refined.The utility model rate of recovery is high, and capacity usage ratio is high, and feed liquid circulation amount is small, and low energy consumption, and no third component is added.
Description
Technical field
The utility model is related to a kind of reclamation set of fusel oil and the process units of ammonia from coal, belong to infiltration evaporation
Technical field.
Background technology
Methanol is important one of basic organic；The production of methanol at present is mainly synthetic method, and the chemistry of synthesis is anti-
Ying Shiwei：2H2+CO→CH3OH, raw material are mainly derived from oil and gas.In recent years, with the valence of oil and gas
The Continued of lattice, coal chemical industry are gradually paid close attention to, and purify to obtain synthesis gas by coal gasification, and deacidification is washed away by low-temp methanol
Property gas after for synthesize obtain crude carbinol.
In the typical process of crude carbinol separation and purification, frequently with four tower separation and purification flows：Including pre-rectifying tower, pressurization
Rectifying column, atmospheric distillation tower and methanol distillation column.Crude carbinol enters pre-rectifying tower, pre-rectifying tower top spray process water extraction essence
It evaporates, after removing light component（Mainly fixed gas, dimethyl ether etc.）, enter compression rectification after bottom of tower methanol and higher boiling composition pressurization
Tower；The condensed refined methanol of vapour phase of compression rectification tower top enters return tank, and a part flows back as pressurizing tower, a part of conduct
Refined methanol product goes out device；Methanol, higher boiling components, the water of pressurizing tower bottom of tower enter atmospheric tower, and Atmospheric Tower produces refined methanol production
Product, are arranged lateral line withdrawal function below feedboard, and extract is mainly methanol, water and high boiling component, again into methanol distillation column
Methanol is recycled, bottom of tower waste water enters biochemical system processing.Recovery tower is equipped with lateral line withdrawal function low boiling fusel oil, to ensure recovery tower tower
It pushes up total alcohol content requirement, bottom of tower waste water in refined methanol quality and bottom of tower waste water and send biochemical treatment.
The low boiling fusel oil of recovery tower lateral line withdrawal function, component be mainly methanol, isopropyl alkene ether, n-hexane, ethyl alcohol, butanone,
Propyl alcohol, normal heptane, water etc., methanol content is related with synthesis condition, and water content is in 30 ~ 50wt.%.In this part fusel oil, moisture
Son forms a variety of binary, polynary azeotropic mixture with each component, is difficult by moisture removal, and for into one by the way of conventional distillation
Methanol in step recycling fusel oil increases prodigious difficulty.Current common dewatering mostly uses molecular sieve adsorbing and dewatering.Portion
Division technique such as Chinese patent, CN1458260A《Fusel oil molecular sieve gas-phase dehydration method and process for separation and purification》In describe
Being directed to the fusel oil during Ethanol Production by Fermentation, using three tower absorbing process and a treating column to complete fusel some de-
The recycling of the products such as water and ethyl alcohol, normal propyl alcohol, isopropanol, isobutanol.But the technique is to be directed to Ethanol Production by Fermentation process
In fusel oil systems, initial water content relatively stablizes, and impurity is based on alcohols.And molecular sieve adsorption plant steam consumption compared with
Height, occupation area of equipment is big, and complex process, yield is low, and the low boiling fusel oil being not appropriate in being produced for ammonia from coal.
In addition, if to fusel oil using the way of distillation recycle methanol when, due in fusel oil contain more water（30-
50%）, water can with other impurity formed azeotropic mixture, make distillation process recycle methanol in can not preferably with other components
Separation keeps the middle impurity content of recycling methanol high.
Invention content
The utility model solve the technical issues of be：The fusel oil generated during ammonia from coal is not easily recycled, passes through steaming
It is high that methanol contaminant content is recycled caused by there is a problem of of water when evaporating method recycling methanol.The skill that the utility model uses
Art design is Pervaporation Technology to be utilized to remove the moisture in fusel oil, then carry out the distillation of methanol by the method for distillation
Recycling, making removal process, low energy consumption, avoid water with impurity azeotropic, improves the purity of recycling methanol.
Technical solution is：
A kind of reuse method of fusel oil, includes the following steps：
1st step, the fusel oil generated in ammonia from coal technique first carry out evaporation and concentrating；
2nd step, the fusel oil after the concentrate obtained to the 1st step are dehydrated by infiltrating and vaporizing membrane；
3rd step, the dehydration fusel oil obtained to the 2nd step are refined using distillating method, are recycled methanol.
Be in 1st step, in the 1st step fusel oil be from refined methanol workshop section methanol distillation column side line take out
Go out, the water content of fusel oil is in 30~70 wt.%.
In 1st step, 10~30 wt.% of water content in the fusel oil after concentrate.
In 1st step, concentration process tower top is flowed back using vapor portion, and reflux ratio is 0.1~10.
In 2nd step, 0.01~3wt.% of water content after dehydration in fusel oil.
In 2nd step, the gauge pressure of the feed liquid side of infiltrating and vaporizing membrane is 0~0.6 MPa；Per-meate side absolute pressure be 50~
2000 Pa。
In 2nd step, infiltration evaporation membrane material is preferential water permeable membrane, such as NaA molecular sieve membrane, PVA film.
In 2nd step, the 1st step concentrate step is returned after the infiltration liquid condensing of infiltrating and vaporizing membrane.
In 3rd step, the rectifying tower bottom temperature range refined in methanol is 105~110 DEG C, tower top temperature range
It it is 65~75 DEG C, 0.04~0.06MPa of pressure, feeding temperature is 75~80 DEG C.
In 1st step, the steam that concentrate obtains is re-fed into the 2nd step infiltration vapour by film absorption process removal hydrogen sulfide
Change.
A kind of reclamation set of fusel oil, including：
Concentration tower 2, for carrying out concentrate to fusel oil；
Segregator 3 is connected to 2 top of concentration tower, for flowing back after the overhead vapor partial condensation to concentration tower 2；
Heating device is connect with the gaseous phase outlet of segregator 3, for being heated to steam；
Pervaporation membrane separator 5, is connected to heating device, for being dehydrated to steam；
Treating column is connected to Pervaporation membrane separator 5, and the distillation for carrying out methanol to dewatered steam is refined.
Further include：
Preheater 1 is connected to concentration tower 2, for being heated to the fusel oil for entering concentration tower 2.
Penetrating fluid condenser 6 is connected to Pervaporation membrane separator 5, is condensed for the penetrating fluid to infiltration evaporation.
Vacuum pump set 7 is connected to Pervaporation membrane separator 5, for making the per-meate side of Pervaporation membrane separator 5 be formed
Vacuum.
The heating device is superheater 4 or heat pump 9.
Film absorber 10 is connected between heating device and penetrating fluid condenser 6, for carrying out removing vulcanization to steam
Hydrogen.
What is installed in the Pervaporation membrane separator 5 is preferential water permeable membrane, such as NaA molecular sieve membrane, PVA film.
A kind of production technology of ammonia from coal, includes the following steps：
It uses coal as raw material and methyl methanol syngas is made, under the effect of the catalyst after synthesizing methanol, methanol is passed through into essence
It evaporates and is refined, the fusel oil produced in distillation process is handled using above-mentioned reuse method.
A kind of process units of ammonia from coal, includes the reclamation set of above-mentioned fusel oil, further includes：
Reactor carries out catalyzing and synthesizing methanol for passing through methanol-fueled CLC system；
Rectifying column is connected to reactor, and rectifying is carried out for the methanol to synthesis；
The side take-off mouth of rectifying column is connected to concentration tower 2.
A method of fusel oil distilation purity is improved, is included the following steps：After fusel oil concentrate, it is sent into infiltration
Vapourizing unit is dehydrated, then dehydration fusel oil is sent into distilation steps processing.
Advantageous effect
1. the utility model is dehydrated using rectifying-Pervaporation membrane separator-rectifying coupling technique, not by azeotropic
Limitation is not required to addition third component, is a kind of isolation technics of high-efficiency environment friendly；
2. the utility model Pervaporation membrane separator high degree of automation, easy to operate, occupation area of equipment is few；
3. penetrating fluid is returned to concentration tower and is recycled by the utility model, reduces the discharge capacity of organic matter, improved
The rate of recovery of machine object；
4, the utility model concentration tower overhead vapor phase is mutually directly entered film device, compared with traditional handicraft, energy saving 30% with
On.
5. the utility model is not condensed by infiltration evaporation product, enters treating column in vapour form, improve in system
Capacity usage ratio further reduced the heating load for the treatment of column.
Description of the drawings
Fig. 1 is that the flow of the dehydration recovery process of low boiling fusel oil in the ammonia from coal production used in Examples 1 and 2 is shown
It is intended to.
Fig. 2 is that the flow of the dehydration recovery process of low boiling fusel oil in the ammonia from coal production used in embodiment 3 and 4 is shown
It is intended to.
Fig. 3 is the flow signal of the dehydration recovery process of low boiling fusel oil in the ammonia from coal production used in embodiment 5
Figure.
Wherein, 1, preheater；2, concentration tower；3, segregator；4, superheater；5, Pervaporation membrane separator；6, penetrating fluid
Condenser；7, vacuum pump set；8, treating column；9, heat pump；10, film absorber.
Specific implementation mode
The utility model is described in further detail below by specific implementation mode.But those skilled in the art will
Understand, the following example is merely to illustrate the utility model, and should not be regarded as limiting the scope of the utility model.In embodiment not
Indicate particular technique or condition person, according to technology or condition described in document in the art or according to product description into
Row.Reagents or instruments used without specified manufacturer, being can be with conventional products that are commercially available.In this specification
" removal ", it further includes the case where part removes (amount for reducing the substance) the case where completely removing target substance to include not only.This
" purification " in specification, including remove arbitrary or specific impurity.
It should be understood that when an element is mentioned with another element " connection ", it can be direct with other elements
It is connected or is indirectly connected with other elements, and inserted with element between them.Unless there are clearly opposite explanation, otherwise term
It includes listed element that " comprising " and " having ", which is interpreted as statement, and non-excluded arbitrary other elements.Word used herein
What language "include", "comprise", " having " or its any other variant were intended to cover non-exclusionism includes.E.g., including it lists and wants
Technique, method, article or the equipment of element are not necessarily limited by those elements, but may include that other are not explicitly listed or belong to
This technique, method, article or the intrinsic element of equipment.Unless the context clearly dictates, otherwise singulative "/kind " and
" (being somebody's turn to do) " includes a plurality of discussion objects.
The utility model to be treated is obtained fusel oil in ammonia from coal, it is generally the case that fusel oil contains
Water is in 30~70 wt.%；The processing method of the utility model by being distilled and concentrated to fusel oil, on the one hand may be used first
So that moisture therein significantly reduces, on the other hand, the heavy constituents such as long chain alkane therein are fallen in removing, after concentrate
Water content in fusel oil can reach 10~30 wt.%；The steam that concentration process generates can carry out partial reflux, and part is steamed
Vapour again by heating after, be sent into infiltration evaporation processing, reflux ratio may be controlled to 0.1~10, during infiltration evaporation
The moisture in concentrate steam can continuously and stably be removed, make to be not easily formed in distilling subtractive process water and other alcohols it
Between azeotropic mixture, avoid the not high problem of recycling methanol purity；The gauge pressure of the feed liquid side of infiltrating and vaporizing membrane is 0~0.6 MPa；
Per-meate side absolute pressure is 50~2000 Pa, and infiltration evaporation membrane material is preferential water permeable membrane, such as NaA molecular sieve membrane, PVA film, infiltration
The 1st step concentrate step is returned after vaporizing the infiltration liquid condensing of film.The dehydration fusel oil that infiltration evaporation obtains, be sent into treating column in into
Row refinement treatment, rectifying tower bottom temperature range are 105~110 DEG C, and tower top temperature range is 65~75 DEG C, pressure 0.04~
0.06MPa, feeding temperature are 75~80 DEG C, in addition, due to containing the sulphur-containing substances such as certain hydrogen sulfide in fusel oil, due to
Its boiling point is relatively low, be easy to cause in the methanol of recycling contain foul smelling, in addition, due between hydrogen sulfide and NaA molecular sieve have compared with
Strong suction-operated is easy to cause molecular screen membrane alcohol-water separation factor in During Process of Long-term Operation and declines, and conventional alkali cleaning
Method material system in this application is simultaneously not suitable for, and is directly resulted in alcohols and is dissolved in lye.It can be absorbed by film
Method handles concentration tower steam, due to being directly to use steam feed in film absorption process, can keep concentrate
The state of steam, and in film absorption process and there is no steam to be in direct contact with liquid, alcohols material can also be avoided direct
The problem of being dissolved in absorbing liquid, being dissolved to avoid the alcohol that direct alkali cleaning is brought；In film absorption process, what be may be used is
Ceramic membrane walks absorbing liquid as film absorber material, such as tubular ceramic membrane inside membrane tube, and shell one sidles concentrate steam, steams
Hydrogen sulfide in vapour contacts to form absorption process with absorbing liquid by fenestra, and alkaline matter can be added in absorbing liquid and improve absorption
Effect, in a preferred embodiment, the absorbing liquid of use is isooctane, it does not dissolve each other with methanol, can to avoid methanol into
Enter absorbing liquid, while can also sponge a part of alkane in steam by compatibility, can have 1 in absorbing liquid with redisperse~
The organic base of 3wt%（Such as amylamine）, the absorptivity for improving hydrogen sulfide, absorbing liquid temperature can be 30~35 DEG C, and concentrate is steamed
Stripping temperature can be 70~90 DEG C, and the average pore size of ceramic membrane can be 50nm.
Based on above technique, the utility model additionally provides the fusel oil reclamation set used, as shown in Figure 1 or 2,
Including：
Concentration tower 2, for carrying out concentrate to fusel oil；
Segregator 3 is connected to 2 top of concentration tower, for flowing back after the overhead vapor partial condensation to concentration tower 2；
Heating device is connect with the gaseous phase outlet of segregator 3, for being heated to steam；
Pervaporation membrane separator 5, is connected to heating device, for being dehydrated to steam；
Treating column is connected to Pervaporation membrane separator 5, and the distillation for carrying out methanol to dewatered steam is refined.
Further include：
Preheater 1 is connected to concentration tower 2, for being heated to the fusel oil for entering concentration tower 2.
Penetrating fluid condenser 6 is connected to Pervaporation membrane separator 5, is condensed for the penetrating fluid to infiltration evaporation.
Vacuum pump set 7 is connected to Pervaporation membrane separator 5, for making the per-meate side of Pervaporation membrane separator 5 be formed
Vacuum.
The heating device is superheater 4 or heat pump 9.
What is installed in the Pervaporation membrane separator 5 is preferential water permeable membrane, such as NaA molecular sieve membrane, PVA film.
As shown in figure 3, further including film absorber 10, it is connected between heating device and penetrating fluid condenser 6, for steaming
Vapour carries out removing hydrogen sulfide.
Based on above technique and method, when can also be applied to during ammonia from coal, integrated work can be formed
Skill route and device.
The production technology of ammonia from coal, including step：It uses coal as raw material and methyl methanol syngas is made, in the work of catalyst
After lower synthesizing methanol, methanol is refined by rectifying, above-mentioned reuse is used to the fusel oil produced in distillation process
Method is handled.
The process units of ammonia from coal includes the reclamation set of above-mentioned fusel oil, further includes：Reactor, for passing through
Methanol-fueled CLC system carries out catalyzing and synthesizing methanol；Rectifying column is connected to reactor, and rectifying is carried out for the methanol to synthesis；Rectifying
The side take-off mouth of tower is connected to concentration tower 2.
Fusel oil derives from the crude carbinol rectifying section of ammonia from coal in following embodiment, at being grouped as（Weight percent）
Including：Methanol 31.4%, isopropyl alkene ether 0.3%, n-hexane 0.9%, ethyl alcohol 6.3%, butanone 0.9%, propyl alcohol 0.8%, butanol 1.1%, just
Heptane 0.5%, hendecane 0.3%, hydrogen sulfide 0.11%, water 46%.
Embodiment 1
The device of use, as shown in Figure 1, fusel oil feed liquid, from after methanol distillation column lateral line withdrawal function, preheated device 1 is preheated to
Entering 2 rectifying concentrate of concentration tower after 82 DEG C, tower top obtains the fusel oil vapour after concentrate, after 3 partial condensation 50% of segregator,
Remaining after superheater 4 is superheated to 120 DEG C enter Pervaporation membrane separator 5 be dehydrated, Pervaporation membrane separator 5 using
The operating pressure of NaA molecular sieve membrane, feed liquid side is 0.25MPa（Gauge pressure）, under the suction of vacuum pump set 7, per-meate side absolute pressure
1000Pa obtains fusel oil dehydration finished product after osmotic, evaporating and dewatering, and the penetrating fluid of removing is after the condensation of penetrating fluid condenser 6
It is back to the recycling of concentration tower 2.Fusel oil is dehydrated the not condensed feeding treating column 8 of finished product steam and refines, 8 operating pressure for the treatment of column
0.06MPa, rectifying column column bottom temperature are 107 DEG C, and tower top temperature is 68 DEG C, and feeding temperature is 77 DEG C, and tower top steams methanol finished product,
Bottom of tower extraction raffinate sends to further separation and recovery.Under the conditions of the operating pressure of different concentration towers 2, obtained operation data is such as
Under：
| Stripper operating pressure MPa | 0.15 | 0.20 | 0.25 | 0.30 |
| Concentrate steam water content wt% | 16.4 | 14.2 | 14.2 | 15.3 |
| Infiltrating and vaporizing membrane runs 0~10h average water fluxs kg/m2·h | 0.91 | 0.93 | 0.96 | 0.90 |
| Infiltrating and vaporizing membrane runs 100~150h average water fluxs kg/m2·h | 0.76 | 0.82 | 0.84 | 0.73 |
| Infiltrating and vaporizing membrane runs 100~150h and is averaged methanol/water separation factor | 773 | 827 | 813 | 796 |
| Recycle methanol content wt% | 91.3 | 95.4 | 95.3 | 92.4 |
| Recycle methanol H2S contents wt% | 0.04 | 0.04 | 0.03 | 0.04 |
Embodiment 2
The device of use, as shown in Figure 1, fusel oil feed liquid, from after methanol distillation column lateral line withdrawal function, preheated device 1 is preheated to
Enter 2 rectifying concentrate of concentration tower, concentration tower operating pressure 0.20MPa after 88 DEG C, tower top obtains the fusel oil vapour after concentrate, passes through
After 3 partial condensation 35% of segregator, remaining enters Pervaporation membrane separator 5 after superheater 4 is superheated to 115 DEG C and is dehydrated, infiltration
Vaporization membrane separator 5 is using NaA molecular sieve membrane, under the suction of vacuum pump set 7, per-meate side absolute pressure 1500Pa, by oozing
The fusel oil dehydration finished product obtained after saturating evaporating and dewatering, the penetrating fluid of removing are back to concentrate after the condensation of penetrating fluid condenser 6
Tower 2 recycles.Fusel oil is dehydrated the not condensed feeding treating column 8 of finished product steam and refines, 8 operating pressure 0.06MPa for the treatment of column, rectifying
Tower column bottom temperature is 107 DEG C, and tower top temperature is 69 DEG C, and feeding temperature is 77 DEG C, and tower top steams methanol finished product, and bottom of tower produces raffinate
Send to further separation and recovery.Under the conditions of the operating pressure of different concentration towers 2, obtained operation data is as follows：
| Infiltrating and vaporizing membrane feed liquid lateral pressure MPa | 0.15 | 0.20 | 0.25 | 0.30 |
| It is dehydrated fusel oil water content wt% | 0.45 | 0.50 | 0.70 | 0.96 |
| Infiltrating and vaporizing membrane runs 0~10h average water fluxs kg/m2·h | 0.86 | 0.97 | 0.95 | 0.89 |
| Infiltrating and vaporizing membrane runs 100~150h average water fluxs kg/m2·h | 0.68 | 0.89 | 0.86 | 0.83 |
| Infiltrating and vaporizing membrane runs 100~150h and is averaged methanol/water separation factor | 769 | 812 | 798 | 786 |
| Recycle methanol content wt% | 92.3 | 95.2 | 96.2 | 93.3 |
Embodiment 3
The device of use, as shown in Figure 1, fusel oil feed liquid, from after methanol distillation column lateral line withdrawal function, preheated device 1 is preheated to
Entering 2 rectifying concentrate of concentration tower after 78 DEG C, tower top obtains the fusel oil vapour after concentrate, after 3 partial condensation 60% of segregator,
Remaining after heat pump 9 is superheated to 125 DEG C enter Pervaporation membrane separator 5 be dehydrated, Pervaporation membrane separator 5 using
The operating pressure of NaA molecular sieve membrane, feed liquid side is 0.25MPa（Gauge pressure）, under the suction of vacuum pump set 7, per-meate side absolute pressure
2000Pa obtains fusel oil dehydration finished product after osmotic, evaporating and dewatering, and the penetrating fluid of removing is after the condensation of penetrating fluid condenser 6
It is back to the recycling of concentration tower 2.Fusel oil is dehydrated the not condensed feeding treating column 8 of finished product steam and refines, 8 operating pressure for the treatment of column
0.06MPa, rectifying column column bottom temperature are 107 DEG C, and tower top temperature is 68 DEG C, and feeding temperature is 77 DEG C, and tower top steams methanol finished product,
Bottom of tower extraction raffinate sends to further separation and recovery.Under the conditions of the operating pressure of different concentration towers 2, obtained operation data is such as
Under：
| Stripper operating pressure MPa | 0.15 | 0.20 | 0.25 | 0.30 |
| Concentrate steam water content wt% | 16.7 | 14.6 | 14.5 | 15.6 |
| Infiltrating and vaporizing membrane runs 0~10h average water fluxs kg/m2·h | 0.88 | 0.92 | 0.94 | 0.87 |
| Infiltrating and vaporizing membrane runs 100~150h average water fluxs kg/m2·h | 0.75 | 0.79 | 0.83 | 0.72 |
| Infiltrating and vaporizing membrane runs 100~150h and is averaged methanol/water separation factor | 784 | 812 | 834 | 785 |
| Recycle methanol content wt% | 91.8 | 95.1 | 95.8 | 92.6 |
Embodiment 4
The device of use, as shown in Figure 1, fusel oil feed liquid, from after methanol distillation column lateral line withdrawal function, preheated device 1 is preheated to
Enter 2 rectifying concentrate of concentration tower, concentration tower operating pressure 0.20MPa after 88 DEG C, tower top obtains the fusel oil vapour after concentrate, passes through
After 3 partial condensation 45% of segregator, remaining enters Pervaporation membrane separator 5 after heat pump 9 is superheated to 112 DEG C and is dehydrated, and permeates vapour
Change membrane separator 5 is using NaA molecular sieve membrane, under the suction of vacuum pump set 7, per-meate side absolute pressure 1200Pa, by infiltration
The fusel oil dehydration finished product obtained after evaporating and dewatering, the penetrating fluid of removing are back to concentration tower 2 after the condensation of penetrating fluid condenser 6
Recycling.Fusel oil is dehydrated the not condensed feeding treating column 8 of finished product steam and refines, 8 operating pressure 0.05MPa for the treatment of column, rectifying column
Column bottom temperature is 110 DEG C, and tower top temperature is 68 DEG C, and feeding temperature is 77 DEG C, and tower top steams methanol finished product, and bottom of tower extraction raffinate is sent
It goes further to separate and recover.Under the conditions of the operating pressure of different concentration towers 2, obtained operation data is as follows：
| Infiltrating and vaporizing membrane feed liquid lateral pressure MPa | 0.15 | 0.20 | 0.25 | 0.30 |
| It is dehydrated fusel oil water content wt% | 0.76 | 0.45 | 0.59 | 0.86 |
| Infiltrating and vaporizing membrane runs 0~10h average water fluxs kg/m2·h | 0.86 | 0.94 | 0.93 | 0.87 |
| Infiltrating and vaporizing membrane runs 100~150h average water fluxs kg/m2·h | 0.75 | 0.88 | 0.89 | 0.85 |
| Infiltrating and vaporizing membrane runs 100~150h and is averaged methanol/water separation factor | 782 | 768 | 788 | 812 |
| Recycle methanol content wt% | 91.4 | 94.5 | 96.7 | 94.6 |
Embodiment 5
The device of use, as shown in Figure 1, fusel oil feed liquid, from after methanol distillation column lateral line withdrawal function, preheated device 1 is preheated to
Entering 2 rectifying concentrate of concentration tower after 82 DEG C, tower top obtains the fusel oil vapour after concentrate, after 3 partial condensation 50% of segregator,
Remaining enters the absorption for the film absorber progress H2S for being equipped with tubular ceramic membrane array, and tubular ceramic membrane material is zirconium oxide, is put down
Equal aperture 50nm, internal diameter 8mm, outer diameter 12mm walk absorbing liquid in pipe（Isooctane containing 3wt% amylamines, 30 DEG C of temperature）, steam
The shell side of ceramic-film tube is walked, 80 DEG C of vapor (steam) temperature, pressure is normal pressure, and the steam after being absorbed by film is overheated using hot device 4
Enter Pervaporation membrane separator 5 after to 120 DEG C to be dehydrated, Pervaporation membrane separator 5 is using NaA molecular sieve membrane, material
The operating pressure of liquid side is 0.25MPa（Gauge pressure）, under the suction of vacuum pump set 7, per-meate side absolute pressure 1000Pa, by permeating vapour
Fusel oil dehydration finished product is obtained after changing dehydration, the penetrating fluid of removing is back to concentration tower 2 after the condensation of penetrating fluid condenser 6 and returns
It receives.Fusel oil is dehydrated the not condensed feeding treating column 8 of finished product steam and refines, 8 operating pressure 0.06MPa for the treatment of column, rectifying tower
Bottom temperature is 107 DEG C, and tower top temperature is 68 DEG C, and feeding temperature is 77 DEG C, and tower top steams methanol finished product, and bottom of tower extraction raffinate is sent to
Further separation and recovery.Under the conditions of the operating pressure of different concentration towers 2, obtained operation data is as follows：
| Stripper operating pressure MPa | 0.15 | 0.20 | 0.25 | 0.30 |
| Concentrate steam water content wt% | 16.4 | 14.2 | 14.2 | 15.3 |
| Infiltrating and vaporizing membrane runs 0~10h average water fluxs kg/m2·h | 1.04 | 1.07 | 1.11 | 1.03 |
| Infiltrating and vaporizing membrane runs 100~150h average water fluxs kg/m2·h | 0.96 | 0.98 | 0.91 | 0.92 |
| Infiltrating and vaporizing membrane runs 100~150h and is averaged methanol/water separation factor | 810 | 833 | 843 | 825 |
| Recycle methanol content wt% | 93.2 | 96.1 | 95.9 | 94.2 |
| Recycle methanol H2S contents wt% | 0.01 | --- | --- | 0.01 |
Reference examples 1
Difference with embodiment 1 is dehydrated without infiltrating and vaporizing membrane.Fusel oil feed liquid is from methanol distillation column lateral line withdrawal function
Afterwards, 2 rectifying concentrate of concentration tower is entered after preheated device 1 is preheated to 82 DEG C, tower top obtains the fusel oil vapour after concentrate, through fractional condensation
After 3 partial condensation 50% of device, remaining is sent into treating column 8 and refines, 8 operating pressure 0.06MPa for the treatment of column, rectifying column column bottom temperature model
It is 107 DEG C to enclose, and tower top temperature is 68 DEG C, and feeding temperature is 77 DEG C, and tower top steams methanol finished product, and bottom of tower extraction raffinate is sent into one
Step separation and recovery.Under the conditions of the operating pressure of different concentration towers 2, obtained operation data is as follows：
| Stripper operating pressure MPa | 0.15 | 0.20 | 0.25 | 0.30 |
| Concentrate steam water content wt% | 16.4 | 14.2 | 14.2 | 15.3 |
| Recycle methanol content wt% | 84.3 | 85.3 | 82.9 | 83.5 |
| Recycle methanol H2S contents wt% | 0.06 | 0.07 | 0.06 | 0.07 |
As can be seen from the table, it is not used in the process for refining of osmotic, evaporating and dewatering, is easy to cause recycling methanol content not
High problem.
Claims (5)
1. a kind of reclamation set of fusel oil, which is characterized in that including：
Concentration tower（2）, for carrying out concentrate to fusel oil；
Segregator（3）, it is connected to concentration tower（2）Top, for concentration tower（2）Overhead vapor partial condensation after flow back；
Heating device, with segregator（3）Gaseous phase outlet connection, for steam heat；
Pervaporation membrane separator（5）, it is connected to heating device, for being dehydrated to steam；
Treating column is connected to Pervaporation membrane separator（5）, refined for the distillation to dewatered steam progress methanol；
Further include：Preheater（1）, it is connected to concentration tower（2）, for entering concentration tower（2）Fusel oil heated；
Further include：Penetrating fluid condenser（6）, it is connected to Pervaporation membrane separator（5）, for the penetrating fluid of infiltration evaporation into
Row condensation；
Further include：Vacuum pump set（7）, it is connected to Pervaporation membrane separator（5）, for making Pervaporation membrane separator（5）'s
Per-meate side forms vacuum.
2. the reclamation set of fusel oil according to claim 1, which is characterized in that the heating device is superheater
（4）Or heat pump（9）.
3. the reclamation set of fusel oil according to claim 1, which is characterized in that the Pervaporation membrane separator
（5）Middle installation is preferential water permeable membrane.
4. the reclamation set of fusel oil according to claim 3, which is characterized in that the preferential water permeable membrane is NaA points
Sub- sieve membrane or PVA film.
5. a kind of process units of ammonia from coal, which is characterized in that including Claims 1 to 4 any one of them fusel oil
Reclamation set further includes：
Reactor carries out catalyzing and synthesizing methanol for passing through methanol-fueled CLC system；
Rectifying column is connected to reactor, and rectifying is carried out for the methanol to synthesis；
The side take-off mouth of rectifying column is connected to concentration tower（2）.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721184780.5U CN207944039U (en) | 2017-09-15 | 2017-09-15 | A kind of reclamation set of fusel oil and the process units of ammonia from coal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721184780.5U CN207944039U (en) | 2017-09-15 | 2017-09-15 | A kind of reclamation set of fusel oil and the process units of ammonia from coal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN207944039U true CN207944039U (en) | 2018-10-09 |
Family
ID=63703273
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201721184780.5U Active CN207944039U (en) | 2017-09-15 | 2017-09-15 | A kind of reclamation set of fusel oil and the process units of ammonia from coal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN207944039U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108409535A (en) * | 2017-09-15 | 2018-08-17 | 江苏九天高科技股份有限公司 | The production technology and device of a kind of reuse method of fusel oil, ammonia from coal |
-
2017
- 2017-09-15 CN CN201721184780.5U patent/CN207944039U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108409535A (en) * | 2017-09-15 | 2018-08-17 | 江苏九天高科技股份有限公司 | The production technology and device of a kind of reuse method of fusel oil, ammonia from coal |
| CN108409535B (en) * | 2017-09-15 | 2024-01-30 | 江苏九天高科技股份有限公司 | Method for recycling fusel oil, production process and device for preparing methanol from coal |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103224456B (en) | Process and device for refining acetonitrile with a pervaporation method | |
| CN104557529B (en) | A kind of process for purification for n-propyl acetate lactate synthesis and device | |
| JP2008540488A (en) | Construction of a new stripping device for the production of ethylene oxide. | |
| CN110272333B (en) | Method for recovering propylene glycol monomethyl ether | |
| US20170203230A1 (en) | System for the Purification of an Organic Solvent and a Process for the use Thereof | |
| TW201034736A (en) | Apparatus and method for recovery of acetic acid, from an aqueous solution thereof | |
| CN105330514B (en) | A kind of purifying technique of synthesis gas preparing ethylene glycol | |
| CN106866368B (en) | Gas field alcohol-containing sewage methanol recovery device and process based on gas stripping method and vacuum membrane distillation method | |
| CN109369419A (en) | The process and device of triethylamine are separated in a kind of industrial wastes | |
| CN104926653A (en) | Reaction and steam osmotic dehydration coupled ethyl hexanoate synthesizing process and device | |
| JP2011162502A (en) | Method for producing absolute ethanol | |
| CN108530396A (en) | A kind of chloro propylene epoxidation method prepares the product purification method of epoxychloropropane | |
| CN106946654A (en) | A kind of separation method of biomass ethylene glycol | |
| CN105152860A (en) | Method for refining mixed alcohol by rectification-pervaporation coupling process | |
| US4088660A (en) | Method for the separation and recovery of furfural and organic volatile acids, such as acetic acid and formic acid, from the process of preparation of furfural | |
| CN104926655A (en) | Technology and device for diethyl oxalate synthesis through vapor permeation dehydration process | |
| CN103396297B (en) | Thermal coupling energy saving system and operation method for recovering organism from propylene epoxidation reaction wastewater | |
| CN207944039U (en) | A kind of reclamation set of fusel oil and the process units of ammonia from coal | |
| CN104926690A (en) | Method and device for recycling and refining acetonitrile in ceftriaxone sodium synthesis | |
| JP2010523701A (en) | Method and apparatus for recovering dichlorohydrin by co-distillation | |
| CN105218316A (en) | A kind of hollow fiber pervaporation membrane prepares the device and method of dehydrated alcohol | |
| CN104610018B (en) | Method for separating ethanol fermentation liquid | |
| CN103613480B (en) | Device and method for recycling low-concentration organic solvent | |
| CN203419863U (en) | Thermal coupling energy-saving system for reclaiming organic matters from propylene epoxidation waste water | |
| CN108424350A (en) | A kind of technique of purification medicinal ethyl alcohol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |