CN105413218A - Immobilized type ionic liquid catalytic reaction rectification device - Google Patents
Immobilized type ionic liquid catalytic reaction rectification device Download PDFInfo
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- CN105413218A CN105413218A CN201510948314.9A CN201510948314A CN105413218A CN 105413218 A CN105413218 A CN 105413218A CN 201510948314 A CN201510948314 A CN 201510948314A CN 105413218 A CN105413218 A CN 105413218A
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- ionic liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Abstract
The invention relates to an immobilized type ionic liquid catalytic reaction rectification device. The immobilized type ionic liquid catalytic reaction rectification device comprises a rectification tower and a raw material storage groove connected with the rectification tower, wherein fillers and a catalyst fixed layer are arranged in the rectification tower; the rectification tower is provided with a tower top reflowing device and a tower kettle storage groove. The immobilized type ionic liquid catalytic reaction rectification device is characterized in that the rectification tower is connected with the tower top reflowing device and a liquid separation rectification head through an electromagnetic reflux ratio controller; the tower top reflowing device comprises an outer reflowing rectification head and a tower top condenser; the liquid separation rectification head is formed by connecting three pipes which are arrayed in parallel and exist independently, and is controlled through the electromagnetic reflux ratio controller. With the adoption of the device, an esterification and product separation process can be effectively shortened, the production efficiency of an esterified product is improved, a traditional process can be replaced and environment-friendly and efficient reaction rectification is realized.
Description
Technical field
The present invention relates to a kind of chemical engineering experiment device, particularly relate to the ionic liquid-catalyzed reaction and rectification device of a kind of solid-carrying type.
Technical background
Esterification is the very important organic chemical reactions of a class, usually adopts fixed bed reaction still, under certain reaction condition, by alcoholic acid esterification, can synthesize a series of ester type compound, be widely used in the field such as petrochemical industry and energy new material.But at present, the production of ester mostly adopts the concentrated sulfuric acid to make catalyst, equipment corrosion is serious, easily causes environmental pollution; And after esterification terminates, the shortcomings such as target product is more difficult with being separated of reactant, there is subsequent treatment complexity, and energy consumption is large.
Ionic liquid, as a kind of new catalyst, has been widely used in chemical reaction.Song Hang etc. are disclose one " preparation of temperature sensitive acidic ionic liquid and the method for catalytic hydroxy acid esterifying thereof " in 201010211280.2 at application number, benzothiazole salt temperature sensitive acidic ionic liquid prepared by the method is in catalytic hydroxy acid esterifying reaction, ionic liquid has highly acid, the feature such as have good stability, but the ionic liquid used synthesis is complicated, and there is the separation of catalyst difficulty, the problems such as post processing more complicated.In recent years, by ionic liquid supported on suitable carrier, solid-carrying type ionic liquid had been prepared.Zhao Yajuan etc. disclose in Chinese invention patent CN101664700A " a kind of solid-carrying type ionic-liquid catalyst and its preparation method and application ", and the catalyst described in the method is immobilizedly on carrier have pyridines acidic ion liquid [XPy] HS0
4, carrier is Y-Al
20
3, Si0
2, mesopore molecular sieve etc., be applied to and catalyze and synthesize in diethylene glycol (DEG) reaction, have that catalyst activity is high, the life-span is long, reaction condition gentleness, the features such as production technology is simple.Functionalization solid-carrying type ionic liquid had both maintained the high catalytic property of ionic liquid to reaction, and make again reaction become heterogeneous reaction, catalyst is easily separated, becomes a kind of novel green catalysis material that can substitute traditional catalyst.
The separation of esterification reaction product and reactant is that in Chemical Manufacture, very typical a kind of Liquid-liquid mixing thing is separated.And utilize each component volatilization performance difference in mixed solution to carry out the distillation operation be separated, be industrial the most frequently used means.Rectifying divides by mode of operation to be had: general rectifying and special extract rectification (comprising extracting rectifying, sequence of constant boiling and rectification).
Up till now, be no matter colleges and universities' research or enterprise's laboratory organic products synthesis lab scale, in reaction and separation of products stage, key technology mainly at screening of catalyst, the reduction of appliance arrangement and operating cost, the aspects such as the joint operation of raw material and product separation technology.Traditional esterification reaction tech selects sulfuric acid or solid strong acid to make catalyst, reaction uses fixed bed reaction still, and be separated the main general distillation operation that adopts, up till now, adopt efficient green catalyst, fixed bed reaction, rectifying, a tower chemical engineering experiment device of proposing technical tie-up operations such as heating up in a steamer also not yet are reported.
Summary of the invention
For the multiple characteristic of more good utilisation solid-carrying type ionic-liquid catalyst, organic esterification reaction, continuous rectification separation.The object of the invention is to provide a kind of solid-carrying type ionic liquid-catalyzed reaction and rectification device.This device adopts fixing beds, and 3 tubular type separatory Rectification head of uniqueness, serves fixed bed reaction, rectifying, puies forward one or more synergies such as heating up in a steamer, can realize one and towerly directly obtain high-purity esters product.This reactive distillation column is simple to operate, and product-collecting and detection facility, catalyst recovery is easy, and reusable.In addition, this device can effectively reduce esterification and product separating technique, realizes process optimization, and improving esterification products production efficiency, is that one can substitute traditional handicraft, realizes environmental protection, efficiently reactive distillation new equipment.
The present invention is achieved through the following technical solutions: the ionic liquid-catalyzed reaction and rectification device of solid-carrying type, comprise rectifying column, the raw material storage tank be connected with rectifying column, filler and catalyst fixed bed is had in rectifying column, rectifying column is provided with overhead reflux device and tower reactor storage tank, it is characterized in that: described rectifying column is by electromagnetism reflux ratio controller, and be connected with overhead reflux device and separatory Rectification head, overhead reflux device comprises exteenal reflux Rectification head and overhead condenser; Described separatory Rectification head be by side by side and self-existent 3 pipes connect to form, controlled by electromagnetism reflux ratio controller.
Preferably, described raw material storage tank is connected with rectifying column by pipeline in the present invention, is provided with flowmeter and valve in pipeline; Described tower reactor storage tank is provided with charge door, and rectifying column tower top, tower reactor storage tank, catalyst fixed bed are provided with temperature measuring equipment thermocouple thermometer; Arrange one section of catalyst fixed bed between two sections of packing layers in rectifying column, on tower body, relevant position is provided with multiple charging aperture.
Gating location on described rectifying column tower body is determined according to catalyst fixed bed position.
Described rectifying column tower body peripheral hardware has electrical heating wire attemperator.
Described tower reactor storage tank is provided with heating jacket.
Described temperature measuring equipment is thermocouple thermometer.
Described flow counts spinner flowmeter.
Described rectifying tower body internal diameter is 30mm, and filler is φ 4*10*1 glass helicoid, packing layer total height 1.6m, catalyst fixed bed 0.5m.
Described rectifying column connects meter control cabinet.
Advantage of the present invention and effect are:
1) this device adopts fixing beds, serves fixed bed reaction, rectifying, puies forward one or more synergies such as heating up in a steamer, can realize one and towerly directly obtain high-purity esters product.
2) 3 unique tubular type separatory Rectification head designs, by solenoid control distillation operation reflux ratio, make distillate pipe upper strata high concentration esters product be easy to backflow, and realization response product oil phase, aqueous phase AUTOMATIC ZONING, is easy to be separated, and is convenient to collect.
3) this device used catalyst is solid-carrying type ionic-liquid catalyst, is fixed between rectifying column packing layer, and make catalytic reaction activity good, catalyst amount is few, and easily reclaims.
Accompanying drawing explanation
Fig. 1 is the ionic liquid-catalyzed reactive distillation column structural representation of embodiment of the present invention solid-carrying type.
Fig. 2 is meter control cabinet schematic diagram in embodiment.
In figure, 1 is rectifying column, and 2 is charging aperture, and 3 is temperature-measuring port, 4 is tower reactor storage tank, and 5 is charge door, and 6 is heating jacket, 7 is exteenal reflux Rectification head, and 8 is evacuated tube, and 9 is separatory Rectification head, 10 is condenser, and 11 is electromagnet, and 12 is metal plectrum, 13 is baffle plate, and 14 is raw material storage tank, and 15 is valve, 16 is spinner flowmeter, and 17 is catalyst fixed bed layer, and 18 is meter control cabinet.
Detailed description of the invention
Provide embodiment below so that the invention will be further described.Be necessary to herein means out, following examples can not be interpreted as limiting the scope of the invention, if person skilled in art makes some nonessential improvement and adjustment according to the invention described above content to the present invention, still belong to protection scope of the present invention.
Embodiment
Embodiment device is see accompanying drawing 1, mainly comprise rectifying column 1, the raw material storage tank 14 be connected with rectifying column 1, filler and catalyst fixed bed 17 is had in rectifying column 1, rectifying column 1 is provided with overhead reflux device and tower reactor storage tank 4, its innovation: rectifying column is by electromagnetism reflux ratio controller, and be connected with overhead reflux device and separatory Rectification head 9, overhead reflux device comprises exteenal reflux Rectification head 7 and overhead condenser 10; Described separatory Rectification head 9 be by side by side and self-existent 3 pipes connect to form, operated by electromagnetism reflux ratio controller.
In embodiment, raw material storage tank 14 is connected with rectifying column 1 by pipeline, is provided with spinner flowmeter 16 and valve 15 in pipeline; Tower reactor storage tank is provided with charge door 5, and rectifying column tower top, tower reactor storage tank 4, catalyst fixed bed 17 are provided with temperature measuring equipment thermocouple thermometer (temperature-measuring port 3 by figure); Arrange one section of catalyst fixed bed 17 between two sections of packing layers in rectifying column, on tower body, relevant position is provided with multiple charging aperture 2, and gating location can be determined according to catalyst fixed bed position.Rectifying column tower body peripheral hardware has electrical heating wire to be incubated, and tower reactor storage tank is provided with heating jacket 6.
Embodiment rectifying tower body internal diameter is 30mm, and filler is φ 4*10*1 glass helicoid, packing layer total height 1.6m, catalyst fixed bed 0.5m.
Embodiment device also connects the meter control cabinet 18 known by this field.
Embodiment 1
Reactive distillation flow process as shown in Figure 1.Before experiment starts, in catalyst fixed bed, first fill a certain amount of supported on silica-gel imidazoles p-methyl benzenesulfonic acid ionic liquid ([Hmim] TsO/silicagel), whole block filling glass helical packing φ 4 in packing layer.Check circuit, after pipe fitting valve switch, starts experiment.First open the cooling water of overhead condenser, from tower reactor charge door 5, add butanols, acetic acid mixed liquor 300ml that mol ratio is 1.2:1, and add cyclohexane 10ml and make water entrainer, by additional hot jacket 6 to tower reactor heating, be heated to boiling, so that wetting tower body filler.Suitable adjustment electric heating voltage, keeps infinite reflux in tower, after whole stable system, carries out continuous feed.Open feedstock valve 15 respectively, by spinner flowmeter 16, regulate charge ratio (mole) 1.2:1 of butanols, acetic acid constant, from tower body charging aperture 2(upper feeding mouth) charging, simultaneously by regulating magnet 11 and metal plectrum 12, with separatory Rectification head 9 joint operation of band baffle plate 13, controlling reflux ratio is 3, refluxes in beginning.Overhead product is in collecting pipe after AUTOMATIC ZONING, open the valve of tower top separatory Rectification head 9, high-purity butyl acetate and water can be collected respectively from two combs, open tower reactor charge door 5 and can collect tower reactor distillate, by temperature-measuring port 3, monitor the temperature of tower top, tower reactor and catalyst layer at any time.
At bottom temperature 95 DEG C, acid-alcohol ratio 1.2:1 (mol ratio), cyclohexane 10ml, ionic liquid consumption is 5.6% of reactant gross mass, reaction time 4h, and esterification yield can reach 99.3%.
Embodiment 2
Reactive distillation flow process as shown in Figure 1.Before experiment starts, in catalyst fixed bed, first fill a certain amount of NaY molecular sieve immobilized imidazoles p-methyl benzenesulfonic acid ionic liquid ([Hmim] TsO/NaY), whole block filling glass helical packing φ 4 in packing layer.Check circuit, after pipe fitting valve switch, starts experiment.First open the cooling water of overhead condenser, from tower reactor charge door 5, add butanols, acetic acid mixed liquor 300ml that mol ratio is 1.2:1, and add cyclohexane 10ml and make water entrainer, by additional hot jacket 6 to tower reactor heating, be heated to boiling, so that wetting tower body filler.Suitable adjustment electric heating voltage, keeps infinite reflux in tower, after whole stable system, carries out continuous feed.Open feedstock valve 15 respectively, by spinner flowmeter 16, regulate charge ratio (mole) 1.2:1 of butanols, acetic acid constant, from tower body charging aperture 2(upper feeding mouth) charging, simultaneously by regulating magnet 11 and metal plectrum 12, with separatory Rectification head 9 joint operation of band baffle plate 13, controlling reflux ratio is 2.5, refluxes in beginning.Overhead product is in collecting pipe after AUTOMATIC ZONING, open the valve of tower top separatory Rectification head 9, high-purity butyl acetate and water can be collected respectively from two combs, open tower reactor charge door 5 and can collect tower reactor distillate, by temperature-measuring port 3, monitor the temperature of tower top, tower reactor and catalyst layer at any time.
At bottom temperature 95 DEG C, acid-alcohol ratio 1.2:1 (mol ratio), cyclohexane 10ml, ionic liquid consumption is 5.0% of reactant gross mass, reaction time 4h, and esterification yield can reach 98.1%.
Embodiment 3
Reactive distillation flow process as shown in Figure 1.Before experiment starts, in catalyst fixed bed, first fill a certain amount of SBA-15 immobilized imidazoles p-methyl benzenesulfonic acid ionic liquid ([Hmim] TsO/SBA-15), whole block filling glass helical packing φ 4 in packing layer.Check circuit, after pipe fitting valve switch, starts experiment.First open the cooling water of overhead condenser, from tower reactor charge door 5, add butanols, acetic acid mixed liquor 300ml that mol ratio is 1.2:1, and add cyclohexane 10ml and make water entrainer, by additional hot jacket 6 to tower reactor heating, be heated to boiling, so that wetting tower body filler.Suitable adjustment electric heating voltage, keeps infinite reflux in tower, after whole stable system, carries out continuous feed.Open feedstock valve 15 respectively, by spinner flowmeter 16, regulate charge ratio (mole) 1.2:1 of butanols, acetic acid constant, charging aperture from tower body charging aperture 2() charging, simultaneously by regulating magnet 11 and metal plectrum 12, with separatory Rectification head 9 joint operation of band baffle plate 13, controlling reflux ratio is 3, refluxes in beginning.Overhead product is in collecting pipe after AUTOMATIC ZONING, open the valve of tower top separatory Rectification head 9, high-purity butyl acetate and water can be collected respectively from two combs, open tower reactor charge door 5 and can collect tower reactor distillate, by temperature-measuring port 3, monitor the temperature of tower top, tower reactor and catalyst layer at any time.
At bottom temperature 95 DEG C, acid-alcohol ratio 1.2:1 (mol ratio), cyclohexane 10ml, ionic liquid consumption is 5.5% of reactant gross mass, reaction time 4h, and esterification yield can reach 99.6%.
Embodiment 4
Reactive distillation flow process as shown in Figure 1.Before experiment starts, in catalyst fixed bed, first fill a certain amount of supported on silica-gel imidazoles p-methyl benzenesulfonic acid ionic liquid ([Hmim] TsO/silicagel), whole block filling glass helical packing φ 4 in packing layer.Check circuit, after pipe fitting valve switch, starts experiment.First open the cooling water of overhead condenser, from tower reactor charge door 5, add ethanol, acetic acid mixed liquor 300ml that mol ratio is 1.2:1, and add cyclohexane 10ml and make water entrainer, by additional hot jacket 6 to tower reactor heating, be heated to boiling, so that wetting tower body filler.Suitable adjustment electric heating voltage, keeps infinite reflux in tower, after whole stable system, carries out continuous feed.Open feedstock valve 15 respectively, by spinner flowmeter 16, regulate charge ratio (mole) 1.2:1 of ethanol, acetic acid constant, from tower body charging aperture 2(upper feeding mouth) charging, simultaneously by regulating magnet 11 and metal plectrum 12, with separatory Rectification head 9 joint operation of band baffle plate 13, controlling reflux ratio is 3, refluxes in beginning.Overhead product is in collecting pipe after AUTOMATIC ZONING, open the valve of tower top separatory Rectification head 9, high-purity ethyl acetate and water can be collected respectively from two combs, open tower reactor charge door 5 and can collect tower reactor distillate, by temperature-measuring port 3, monitor the temperature of tower top, tower reactor and catalyst layer at any time.
At bottom temperature 90 DEG C, acid-alcohol ratio 1.2:1 (mol ratio), cyclohexane 10ml, ionic liquid consumption is 5.6% of reactant gross mass, reaction time 4h, and esterification yield can reach 99.5%.
Embodiment 5
Reactive distillation flow process as shown in Figure 1.Before experiment starts, in catalyst fixed bed, first fill a certain amount of NaY molecular sieve immobilized imidazoles p-methyl benzenesulfonic acid ionic liquid ([Hmim] TsO/NaY), whole block filling glass helical packing φ 4 in packing layer.Check circuit, after pipe fitting valve switch, starts experiment.First open the cooling water of overhead condenser, from tower reactor charge door 5, add ethanol, acetic acid mixed liquor 300ml that mol ratio is 1.2:1, and add cyclohexane 10ml and make water entrainer, by additional hot jacket 6 to tower reactor heating, be heated to boiling, so that wetting tower body filler.Suitable adjustment electric heating voltage, keeps infinite reflux in tower, after whole stable system, carries out continuous feed.Open feedstock valve 15 respectively, by spinner flowmeter 16, regulate charge ratio (mole) 1.2:1 of ethanol, acetic acid constant, charging aperture from tower body charging aperture 2() charging, simultaneously by regulating magnet 11 and metal plectrum 12, with separatory Rectification head 9 joint operation of band baffle plate 13, controlling reflux ratio is 2.5, refluxes in beginning.Overhead product is in collecting pipe after AUTOMATIC ZONING, open the valve of tower top separatory Rectification head 9, high-purity ethyl acetate and water can be collected respectively from two combs, open tower reactor charge door 5 and can collect tower reactor distillate, by temperature-measuring port 3, monitor the temperature of tower top, tower reactor and catalyst layer at any time.
At bottom temperature 90 DEG C, acid-alcohol ratio 1.2:1 (mol ratio), cyclohexane 10ml, ionic liquid consumption is 5.0% of reactant gross mass, reaction time 4h, and esterification yield can reach 98.6%.
Embodiment 6
Reactive distillation flow process as shown in Figure 1.Before experiment starts, in catalyst fixed bed, first fill a certain amount of supported on silica-gel imidazoles p-methyl benzenesulfonic acid ionic liquid ([Hmim] TsO/silicagel), whole block filling glass helical packing φ 4 in packing layer.Check circuit, after pipe fitting valve switch, starts experiment.First open the cooling water of overhead condenser, from tower reactor charge door 5, add butanols, propionic acid mixed liquor 300ml that mol ratio is 1.2:1, and add cyclohexane 10ml and make water entrainer, by additional hot jacket 6 to tower reactor heating, be heated to boiling, so that wetting tower body filler.Suitable adjustment electric heating voltage, keeps infinite reflux in tower, after whole stable system, carries out continuous feed.Open feedstock valve 15 respectively, pass through spinner flowmeter, regulate charge ratio (mole) 1.2:1 of butanols, propionic acid constant, from tower body charging aperture 2(upper feeding mouth) charging, simultaneously by regulating magnet 11 and metal plectrum 12, with separatory Rectification head 9 joint operation of band baffle plate 13, controlling reflux ratio is 3, refluxes in beginning.Overhead product is in collecting pipe after AUTOMATIC ZONING, open the valve of tower top separatory Rectification head 9, high-purity butyl propionate and water can be collected respectively from two combs, open tower reactor charge door 5 and can collect tower reactor distillate, by temperature-measuring port 3, monitor the temperature of tower top, tower reactor and catalyst layer at any time.
At bottom temperature 95 DEG C, acid-alcohol ratio 1.2:1 (mol ratio), cyclohexane 10ml, ionic liquid consumption is 5.6% of reactant gross mass, reaction time 4h, and esterification yield can reach 99.1%.
Embodiment 7
Reactive distillation flow process as shown in Figure 1.Before experiment starts, in catalyst fixed bed, first fill a certain amount of SBA-15 immobilized imidazoles p-methyl benzenesulfonic acid ionic liquid ([Hmim] TsO/SBA-15), whole block filling glass helical packing φ 4 in packing layer.Check circuit, after pipe fitting valve switch, starts experiment.First open the cooling water of overhead condenser, from tower reactor charge door 5, add butanols, propionic acid mixed liquor 300ml that mol ratio is 1.2:1, and add cyclohexane 10ml and make water entrainer, by additional hot jacket 6 to tower reactor heating, be heated to boiling, so that wetting tower body filler.Suitable adjustment electric heating voltage, keeps infinite reflux in tower, after whole stable system, carries out continuous feed.Open feedstock valve 15 respectively, by spinner flowmeter 16, regulate charge ratio (mole) 1.2:1 of butanols, propionic acid constant, charging aperture from tower body charging aperture 2() charging, simultaneously by regulating magnet 11 and metal plectrum 12, with separatory Rectification head 9 joint operation of band baffle plate 13, controlling reflux ratio is 3.5, refluxes in beginning.Overhead product is in collecting pipe after AUTOMATIC ZONING, open the valve of tower top separatory Rectification head 9, high-purity butyl propionate and water can be collected respectively from two combs, open tower reactor charge door 5 and can collect tower reactor distillate, by temperature-measuring port 3, monitor the temperature of tower top, tower reactor and catalyst layer at any time.
At bottom temperature 95 DEG C, acid-alcohol ratio 1.2:1 (mol ratio), cyclohexane 10ml, ionic liquid consumption is 5.5% of reactant gross mass, reaction time 4h, and esterification yield can reach 99.7%.
Claims (9)
1. the ionic liquid-catalyzed reaction and rectification device of solid-carrying type, comprise rectifying column, the raw material storage tank be connected with rectifying column, filler and catalyst fixed bed is had in rectifying column, rectifying column is provided with overhead reflux device and tower reactor storage tank, it is characterized in that: described rectifying column is by electromagnetism reflux ratio controller, and be connected with overhead reflux device and separatory Rectification head, overhead reflux device comprises exteenal reflux Rectification head and overhead condenser; Described separatory Rectification head be by side by side and self-existent 3 pipes connect to form, controlled by electromagnetism reflux ratio controller.
2. the ionic liquid-catalyzed reaction and rectification device of solid-carrying type as claimed in claim 1, is characterized in that: described raw material storage tank is connected with rectifying column by pipeline, is provided with flowmeter and valve in pipeline; Described tower reactor storage tank is provided with charge door, and rectifying column tower top, tower reactor storage tank, catalyst fixed bed are provided with temperature measuring equipment thermocouple thermometer; Arrange one section of catalyst fixed bed between two sections of packing layers in rectifying column, on tower body, relevant position is provided with multiple charging aperture.
3. the ionic liquid-catalyzed reaction and rectification device of solid-carrying type as claimed in claim 1, is characterized in that: the gating location on described rectifying column tower body is determined according to catalyst fixed bed position.
4. the ionic liquid-catalyzed reaction and rectification device of solid-carrying type as claimed in claim 1, is characterized in that: described rectifying column tower body peripheral hardware has electrical heating wire attemperator.
5. the ionic liquid-catalyzed reaction and rectification device of solid-carrying type as claimed in claim 1, is characterized in that: described tower reactor storage tank is provided with heating jacket.
6. the ionic liquid-catalyzed reaction and rectification device of solid-carrying type as claimed in claim 1, is characterized in that: described temperature measuring equipment is thermocouple thermometer.
7. the ionic liquid-catalyzed reaction and rectification device of solid-carrying type as claimed in claim 1, is characterized in that: described flow counts spinner flowmeter.
8. the ionic liquid-catalyzed reaction and rectification device of solid-carrying type as claimed in claim 1, it is characterized in that: described rectifying tower body internal diameter is 30mm, filler is φ 4*10*1 glass helicoid, packing layer total height 1.6m, catalyst fixed bed 0.5m.
9. the ionic liquid-catalyzed reaction and rectification device of solid-carrying type as claimed in claim 1, is characterized in that: described rectifying column connects meter control cabinet.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510948314.9A CN105413218A (en) | 2015-12-17 | 2015-12-17 | Immobilized type ionic liquid catalytic reaction rectification device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510948314.9A CN105413218A (en) | 2015-12-17 | 2015-12-17 | Immobilized type ionic liquid catalytic reaction rectification device |
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| CN105413218A true CN105413218A (en) | 2016-03-23 |
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| CN201510948314.9A Pending CN105413218A (en) | 2015-12-17 | 2015-12-17 | Immobilized type ionic liquid catalytic reaction rectification device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109464823A (en) * | 2018-12-29 | 2019-03-15 | 天津天元伟业化工技术有限公司 | Random packing tower for high-precision separation |
| CN116514653A (en) * | 2023-04-21 | 2023-08-01 | 安徽瑞柏新材料有限公司 | Production process of ethyl acetate |
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| CN103752030A (en) * | 2014-01-09 | 2014-04-30 | 沈阳化工大学 | Ionic liquid extractive distillation experiment device |
| CN203677981U (en) * | 2014-01-09 | 2014-07-02 | 沈阳化工大学 | Ionic liquid extractive distillation experimental device |
| CN104548644A (en) * | 2014-12-08 | 2015-04-29 | 南京化工职业技术学院 | Distillation experimental device for supported ionic liquid catalytic reaction |
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| CN1832790A (en) * | 2003-08-05 | 2006-09-13 | 巴斯福股份公司 | Recycling of ionic liquids produced in extractive distillation |
| CN102180791A (en) * | 2011-04-13 | 2011-09-14 | 天津大学 | Method for separating methyl acetate-methanol mixture by ionic liquid intermittent extractive rectification |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109464823A (en) * | 2018-12-29 | 2019-03-15 | 天津天元伟业化工技术有限公司 | Random packing tower for high-precision separation |
| CN116514653A (en) * | 2023-04-21 | 2023-08-01 | 安徽瑞柏新材料有限公司 | Production process of ethyl acetate |
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