CN108246222A - Novel major axis magnetic force pump type reactor - Google Patents

Novel major axis magnetic force pump type reactor Download PDF

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Publication number
CN108246222A
CN108246222A CN201810008798.2A CN201810008798A CN108246222A CN 108246222 A CN108246222 A CN 108246222A CN 201810008798 A CN201810008798 A CN 201810008798A CN 108246222 A CN108246222 A CN 108246222A
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column plate
tower
ranging
gas distributor
liquid
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CN108246222B (en
Inventor
刘肖肖
江继峰
陈迎
裴凯凯
贾微
徐曼
张艺
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Sinopec Engineering Group Co Ltd
Sinopec Shanghai Engineering Co Ltd
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Sinopec Engineering Group Co Ltd
Sinopec Shanghai Engineering Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/32Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • B01J19/0066Stirrers
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/03Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention relates to a kind of novel major axis magnetic force pump type reactors, mainly solve the problems, such as that gas-liquid-solid three-phase mixing is non-uniform in the prior art.The present invention is by using a kind of novel major axis magnetic force pump type reactor, run through in reactor by 1~2 root long axis, long axis is wrapped up by long casing, inside installs bearing additional, make axis, bearing and the medium in outside are completely isolated, the blade impregnated in the medium is coupled with axis using the principle of magnetic drive pump, realize the effect of stirring, every layer of column plate arrangement riser in reactor, riser air inlet is located at reactor long axis side, and connect gas distributor on riser top, gas distributor center is fallen on long axis, gas phase from descending trays is uniformly sprayed by gas distributor in the liquid-solid mixture on column plate, the technical solution that every layer of column plate is equipped with liquid phase disengaging facility preferably solves the above problem, available in gas-liquid-solid three phase catalytic reaction rectifying.

Description

Novel major axis magnetic force pump type reactor
Technical field
The present invention relates to a kind of novel major axis magnetic force pump type reactors.
Background technology
With the rise and development of green chemical industry, chemical process reinforcement technique increasingly attracts attention.Will chemical reaction and Rectifying separation carries out the integrated reaction rectification technique for forming polyfunctional reactant device, be realize approach that chemical process strengthens it One.Catalytic distillation is the heterogeneous catalytic reaction distillation technology to grow up on the basis of homogeneous reaction rectifying, which will be solid Body catalyst is placed in tower on each layer column plate of conversion zone, and gas and liquid distinguish counter-current flow up and down, chemical reaction It detaches with rectifying and is coupled in tower inner height, can constantly remove reaction product, reaction heat also can be as the vaporization of distillation process Heat.Compared to the continuous stirred tank reactor of series connection, catalytic rectifying tower have Low investment, low energy consumption, high conversion, it is highly selective, The advantages that high productive capacity, in etherificate, alkylation, ether solution, ester hydrolysis, esterification, transesterification, dimerization plus hydrogen, isomerization, de- It is applied in the chemical processes such as water.For gas-liquid-solid three-phase catalytic distillation existing for solid particle or particulate catalyst, respectively The uniform mixing of gas-liquid-solid three-phase is difficult point between column plate, is adapted for continuously stirring, be uniformly mixed and safe and reliable catalysis essence The design for evaporating tower is very necessary.
101618304 A of patent CN describe a kind of esterifier, by connecting rotatable gas on riser top Body distributor, on each layer column plate can carry out gas-liquid-solid three-phase continuously stirs, but be limited to the power that gas flow rate is brought, solid Beaded catalyst does not ensure that stirring is abundant on every layer of column plate, is uniformly mixed.
1015175211 A of patent CN propose the high-purity isobutene of tert-butyl alcohol dehydration system using window diversion type structured packing Catalytic distillation is carried out, method is simple, effect is good, but catalyst change is difficult, it is desirable that catalyst has a longer life expectancy.
105561911 A of patent CN propose catalyst in a kind of efficient catalytic rectifying column and tie up filler and its preparation side Method, catalyst packet is interior to be fitted closely equipped with solid catalyst particle, the catalyst packet chain and regular corrugation filler piece after spiraling It is fixed-type by lock ring piece.The catalyst packet hollow structure of the patented invention increases gas-liquid mass transfer space, can effectively facilitate anti- The progress answered, but catalyst change is difficult, and generally requiring parking could replace, more demanding to catalyst life.
101219950 A of patent CN give a kind of ester exchange reaction using methyl acetate and n-butanol and prepare acetic acid The system and method for N-butyl, the catalytic rectifying tower are made of stripping section, conversion zone, rectifying section, and wherein conversion zone is by liquid collecting Plate, riser, catalyst packet, support plate and bottom plate are formed, easy to operate, methyl acetate high conversion rate, but catalyst packet is replaced It is difficult.
Patent CN 205731266 discloses a kind of autoclave blender, using the mixing blade of double belt screw structures, stirs It mixes more thoroughly, improves stirring efficiency and effect, but agitating paddle bearing and transmission shaft are often corroded rapidly, cause frequently Maintenance increases maintenance cost.
Invention content
The technical problems to be solved by the invention are that gas-liquid-solid three-phase mixes non-uniform problem in the prior art, provide one The new novel major axis magnetic force pump type reactor of kind.The reactor has the advantages that gas-liquid-solid three-phase is uniformly mixed.
To solve the above problems, the technical solution adopted by the present invention is as follows:A kind of novel major axis magnetic force pump type reactor, instead It answers and is run through in device by 1~2 root long axis, long axis is wrapped up by long casing, and inside installs bearing additional, makes axis, bearing and the medium in outside complete Full isolation is coupled the blade impregnated in the medium with axis using the principle of magnetic drive pump, realizes the effect of stirring, in reactor often Layer column plate arrangement riser, riser air inlet is located at reactor long axis side, and connects gas distributor on riser top, Gas distributor center is fallen on long axis, and the liquid that the gas phase from descending trays is uniformly sprayed by gas distributor on column plate is consolidated In mixture, every layer of column plate is equipped with liquid phase disengaging facility, and liquid phase feeding mouth and liquid-phase outlet, column plate are set respectively in column plate both sides Liquid phase enters descending trays outside tower or downspout is set on column plate, and liquid phase flows to lower floor's tower by upper strata column plate in tower Plate;Solid particle or particulate catalyst are placed on every layer of column plate, and catalyst loading and unloading mouth is equipped on every layer of column plate of reactor, Can under the conditions of not parking more catalyst changeout;Wherein, adjacent two pieces of column plate spacing be H, tower internal diameter be D, H ranging from 300~ 700mm;Gas distributor outer tube opening diameter ranging from 2~25mm, inner tube opening diameter ranging from 1~20mm, between trepanning Equidistantly it is uniformly distributed;The ratio between the draft tube diameter c and tower internal diameter D ranging from 0.05~0.25, riser import center and tower Plate centre distance ranging from 0.1~0.3D, the ratio between the descending liquid pipe diameter d and tower internal diameter D ranging from 0.08~0.25, the drop Liquid pipe center line is away from column plate centre distance ranging from 0.20~0.45D, and the downspout must stretch into tower tray liquid level hereinafter, downspout The ratio between height h and adjacent two pieces of column plate spacing H ranging from 0.4~0.9.
In above-mentioned technical proposal, it is preferable that be furnished with strainer at liquid-phase outlet or downcomer inlet, prevent under catalyst entrance Layer column plate.
In above-mentioned technical proposal, it is preferable that the gas distributor is ring type gas distributor.
In above-mentioned technical proposal, it is highly preferred that gas distributor is dicyclic gas distributor, the dicyclic gas point The ratio between cloth device outer tube diameter a and tower internal diameter D are 0.3~0.8, and the ratio between interior caliber b and tower internal diameter D are 0.2~0.7, dicyclic gas Distributor center is overlapped with column plate center.
In above-mentioned technical proposal, it is preferable that adjacent two pieces of column plate spacing be H, tower internal diameter be D, H ranging from 400~ 600mm;Gas distributor outer tube opening diameter ranging from 5~20mm, inner tube opening diameter ranging from 5~15mm, between trepanning Equidistantly it is uniformly distributed;The ratio between the draft tube diameter c and tower internal diameter D ranging from 0.1~0.15;Riser import center and column plate Centre distance ranging from 0.1~0.2D;The ratio between the descending liquid pipe diameter d and tower internal diameter D ranging from 0.1~0.15;The descending liquid Tube hub line-spacing column plate centre distance ranging from 0.3~0.4D;The ratio between the downspout height h and adjacent two pieces of column plate spacing H Ranging from 0.6~0.8.
In above-mentioned technical proposal, it is preferable that magnetic force Pump-like stirrer is equipped in reactor.
In above-mentioned technical proposal, it is preferable that medium is gas-liquid-solid three-phase.
The present invention mixes problem of non-uniform to solve in existing catalytic rectifying tower gas-liquid-solid three-phase between column plate, provides one kind Novel major axis magnetic force pump type reactor.The reactor has gas-liquid-solid three-phase good mixing effect, isolation axis and bearing, magnetic agitation The features such as reliable;Solid particle or particulate catalyst are placed on every layer of column plate, since density of solid and liquid approach, Suspended dispersed is in liquid phase under the action of agitating paddle for solid catalyst, so gas-liquid-solid three-phase stirring is abundant in reaction unit, It is uniformly mixed, reaction efficiency is good.Catalyst loading and unloading mouth is equipped on every layer of column plate of simultaneous reactions device, it can be under the conditions of not parking more Catalyst changeout.The present invention has the characteristics that can to continuously stir, gas-liquid-solid three-phase is uniformly mixed, structure is safe and reliable, stable, Achieve preferable technique effect.
Description of the drawings
Fig. 1 is one of structure diagram of reactor of the present invention, only illustrates tower adjacent two pieces of tower plate structures topmost.
In Fig. 1,1 magnetic-type blender, 2 long axis, 37 liters of 5 heavy constituent feed inlet of long 4 blade of axle sleeve, 6 gas distributor 14 column plate of tracheae 8 fluid inlet, 9 catalyst make-up mouth, 10 column plate, 11 tower body, 12 strainer, 13 liquid-phase outlet, 15 liquid phase goes out 16 catalyst outlets of mouth.
Fig. 2 is the second structural representation of reactor of the present invention, only illustrates tower adjacent two pieces of tower plate structures topmost.
In Fig. 2,1 magnetic-type blender, 2 long axis, 37 liters of 5 heavy constituent feed inlet of long 4 blade of axle sleeve, 6 gas distributor 13 downspout of tracheae 8 tower body, 9 catalyst make-up mouth, 10 column plate, 11 strainer, 12 column plate, 14 catalyst outlet.
Fig. 3 is that with n-butanol ester-interchange method butyl acetate reactive distillation processes flow occurs for methyl acetate in embodiment Schematic diagram.
In Fig. 3,1 catalytic rectifying tower, 2 condenser, 3 return tank, 4 reboiler, 5 reflux pump.
The present invention will be further described below by way of examples, but is not limited only to the present embodiment.
Specific embodiment
【Embodiment 1】
A kind of novel major axis magnetic force pump type reactor, as shown in Figure 1, being run through in reactor by 1 root long axis, long axis is by growing set Pipe wraps up, and inside installs bearing additional, makes axis, bearing and the medium in outside completely isolated, Jie will be immersed in using the principle of magnetic drive pump Blade in matter is coupled with axis, realizes the effect of stirring, and every layer of column plate arrangement riser, riser air inlet are located in reactor Reactor long axis side, and gas distributor is connected on riser top, gas distributor center is fallen on long axis, from lower floor The gas phase of column plate is uniformly sprayed by gas distributor in the liquid-solid mixture on column plate, and every layer of column plate is equipped with liquid phase disengaging and sets It applies, sets liquid phase feeding mouth and liquid-phase outlet respectively in column plate both sides, column plate liquid phase enters descending trays outside tower;Solid particle or Particulate catalyst is placed on every layer of column plate, and catalyst loading and unloading mouth is equipped on every layer of column plate of reactor, can be in not parking item More catalyst changeout under part;Wherein, adjacent two pieces of column plate spacing are H, and tower internal diameter is D, H 450mm;Gas distributor outer tube trepanning A diameter of 12mm, inner tube opening diameter are 8mm, are equidistantly uniformly distributed between trepanning;The draft tube diameter c and tower internal diameter D it Than being 0.1, riser import center is 0.2D with column plate centre distance, and the ratio between the descending liquid pipe diameter d and tower internal diameter D are 0.12, the downspout center line is 0.4D, the downspout height h and adjacent two pieces of column plate spacing H away from column plate centre distance The ratio between be 0.7.Gas distributor is dicyclic gas distributor, the dicyclic gas distributor outer tube diameter a and tower internal diameter D it Than being 0.5, the ratio between interior caliber b and tower internal diameter D are 0.4, and dicyclic gas distributor center is overlapped with column plate center.
By taking ester-interchange method butyl acetate reactive distillation processes occur for methyl acetate and n-butanol as an example, as shown in Figure 3. Specific implementation process is as follows:10 blocks of column plates, pattern such as Fig. 2, tower internal diameter 200mm are installed in catalytic rectifying tower (1).Each layer tower Transesterification is filled on plate and dissipates heap granular pattern catalyst.N-butanol feeds (101) into the 2nd block of column plate of catalytic rectifying tower (1), vinegar Sour methyl esters feeds (102) into the 10th block of column plate of catalytic rectifying tower (1).Methyl acetate and n-butanol counter current contacting, and occur anti- It should be with detaching.Overhead vapours (103) main component is methyl acetate and methanol, is condensed into condenser (2), lime set (105) into return tank (3), return tank liquid phase discharging (106) passes through reflux pump (5) partial reflux (107) to catalytic rectifying tower (1), into later separation workshop section, the methyl acetate after separation is recycled to catalytic rectifying tower (1) into traveling for part extraction (110) One step ester exchange reaction.Catalytic rectifying tower (1) tower reactor be equipped with reboiler provide heat source, tower reactor main component for n-butyl acetate with Later separation and refinement are gone in n-butanol, tower reactor extraction (104), to obtain n-butyl acetate product, while the positive fourth recycled Alcohol is recycled to catalytic rectifying tower (1) and further ester exchange reaction occurs.
Using the novel major axis magnetic force pump type reactor of the present invention as catalytic distillation device, as methyl acetate and n-butanol Transesterification catalytic rectifying tower (1).Tower top operation temperature is 75 DEG C, and tower top operating pressure is 0.12MPa (A).N-butanol feeds (1) (2) molar ratio=2 are fed with methyl acetate:1, mass flow is respectively:75kg/h, 38.3kg/h, reflux ratio 12 carry out Continuous experiment, during stable operation, methyl acetate conversion per pass is up to 59.5%.
【Embodiment 2】
A kind of novel major axis magnetic force pump type reactor, as shown in Fig. 2, being run through in reactor by 1 root long axis, long axis is by growing set Pipe wraps up, and inside installs bearing additional, makes axis, bearing and the medium in outside completely isolated, Jie will be immersed in using the principle of magnetic drive pump Blade in matter is coupled with axis, realizes the effect of stirring, and every layer of column plate arrangement riser, riser air inlet are located in reactor Reactor long axis side, and gas distributor is connected on riser top, gas distributor center is fallen on long axis, from lower floor The gas phase of column plate is uniformly sprayed by gas distributor in the liquid-solid mixture on column plate, and every layer of column plate is equipped with liquid phase disengaging and sets It applies, downspout is set on column plate, liquid phase flows to descending trays by upper strata column plate in tower;Solid particle or particulate catalyst It is placed on every layer of column plate, catalyst loading and unloading mouth is equipped on every layer of column plate of reactor, catalysis can be replaced under the conditions of not parking Agent;Wherein, adjacent two pieces of column plate spacing are H, and tower internal diameter is D, H 300mm;Gas distributor outer tube opening diameter is 2mm, interior Pipe opening diameter is 1mm, is equidistantly uniformly distributed between trepanning;The ratio between the draft tube diameter c and tower internal diameter D are 0.05, rise gas Pipe import center is 0.1D with column plate centre distance, and the ratio between the descending liquid pipe diameter d and tower internal diameter D are 0.08, the downspout Center line is 0.2D away from column plate centre distance, and the ratio between the downspout height h and adjacent two pieces of column plate spacing H are 0.4.Gas point Cloth device is dicyclic gas distributor, and the ratio between the dicyclic gas distributor outer tube diameter a and tower internal diameter D are 0.3, interior caliber b It is 0.2 with the ratio between tower internal diameter D, dicyclic gas distributor center is overlapped with column plate center.
It is anti-with methyl acetate and n-butanol generation ester-interchange method butyl acetate according to the condition and step of embodiment 1 For answering distillation process, as shown in Figure 3.Specific implementation process is as follows:10 blocks of column plates, type are installed in catalytic rectifying tower (1) Formula such as Fig. 1, tower internal diameter 200mm.Transesterification is filled on each layer column plate and dissipates heap granular pattern catalyst.N-butanol feed (101) into Enter the 2nd block of column plate of catalytic rectifying tower (1), methyl acetate feeds (102) into the 10th block of column plate of catalytic rectifying tower (1).Tumer Ester and n-butanol counter current contacting, and react with detaching.Overhead vapours (103) main component be methyl acetate and methanol, into Enter condenser (2) to be condensed, lime set (105) passes through reflux pump (5) portion into return tank (3), return tank liquid phase discharging (106) Divide reflux (107) to catalytic rectifying tower (1), part produces (110) into later separation workshop section, and the methyl acetate after separation can follow Ring to catalytic rectifying tower (1) carries out further ester exchange reaction.Catalytic rectifying tower (1) tower reactor is equipped with reboiler and provides heat source, tower Kettle main component is n-butyl acetate and n-butanol, and later separation and refinement are gone in tower reactor extraction (104), to obtain acetic acid just Butyl ester product, while the n-butanol recycled is recycled to catalytic rectifying tower (1) and further ester exchange reaction occurs.
Using the novel major axis magnetic force pump type reactor of the present invention as catalytic distillation device, as methyl acetate and n-butanol Transesterification catalytic rectifying tower (1).Tower top operation temperature is 75 DEG C, and tower top operating pressure is 0.12MPa (A).N-butanol feeds (1) (2) molar ratio=2 are fed with methyl acetate:1, mass flow is respectively:75kg/h, 38.3kg/h, reflux ratio 14 carry out Continuous experiment, during stable operation, methyl acetate conversion per pass is up to 58.5%.
【Embodiment 3】
According to condition described in embodiment 1 and step, adjacent two pieces of column plate spacing are H, and tower internal diameter is D, H 400mm;Gas Body distributor outer tube opening diameter is 10mm, and inner tube opening diameter is 8mm, is equidistantly uniformly distributed between trepanning;The riser The ratio between diameter c and tower internal diameter D are 0.1, and riser import center and column plate centre distance are 0.2D, the descending liquid pipe diameter d with The ratio between tower internal diameter D be 0.25, the downspout center line away from column plate centre distance be 0.45D, the downspout height h with it is adjacent The ratio between two pieces of column plate spacing H are 0.7.Gas distributor be dicyclic gas distributor, the dicyclic gas distributor outer tube The ratio between diameter a and tower internal diameter D are 0.5, and the ratio between interior caliber b and tower internal diameter D are 0.4, in dicyclic gas distributor center and column plate The heart overlaps.
By taking ester-interchange method butyl acetate reactive distillation processes occur for methyl acetate and n-butanol as an example, as shown in Figure 3. Specific implementation process is as follows:10 blocks of column plates, pattern such as Fig. 2, tower internal diameter 200mm are installed in catalytic rectifying tower (1).Each layer tower Transesterification is filled on plate and dissipates heap granular pattern catalyst.N-butanol feeds (101) into the 2nd block of column plate of catalytic rectifying tower (1), vinegar Sour methyl esters feeds (102) into the 10th block of column plate of catalytic rectifying tower (1).Methyl acetate and n-butanol counter current contacting, and occur anti- It should be with detaching.Overhead vapours (103) main component is methyl acetate and methanol, is condensed into condenser (2), lime set (105) into return tank (3), return tank liquid phase discharging (106) passes through reflux pump (5) partial reflux (107) to catalytic rectifying tower (1), into later separation workshop section, the methyl acetate after separation is recycled to catalytic rectifying tower (1) into traveling for part extraction (110) One step ester exchange reaction.Catalytic rectifying tower (1) tower reactor be equipped with reboiler provide heat source, tower reactor main component for n-butyl acetate with Later separation and refinement are gone in n-butanol, tower reactor extraction (104), to obtain n-butyl acetate product, while the positive fourth recycled Alcohol is recycled to catalytic rectifying tower (1) and further ester exchange reaction occurs.
Using the novel major axis magnetic force pump type reactor of the present invention as catalytic distillation device, as methyl acetate and n-butanol Transesterification catalytic rectifying tower (1).Tower top operation temperature is 75 DEG C, and tower top operating pressure is 0.12MPa (A).N-butanol feeds (1) (2) molar ratio=2 are fed with methyl acetate:1, mass flow is respectively:75kg/h, 38.3kg/h, reflux ratio 12 carry out Continuous experiment, during stable operation, methyl acetate conversion per pass is up to 58.6%.
【Embodiment 4】
According to condition described in embodiment 1 and step, adjacent two pieces of column plate spacing are H, and tower internal diameter is D, H 500mm;Gas Body distributor outer tube opening diameter is 15mm, and inner tube opening diameter is 10mm, is equidistantly uniformly distributed between trepanning;The riser The ratio between diameter c and tower internal diameter D are 0.15, and riser import center is 0.15D, the descending liquid pipe diameter d with column plate centre distance Be 0.1 with the ratio between tower internal diameter D, the downspout center line is 0.3D away from column plate centre distance, the downspout height h with it is adjacent The ratio between two pieces of column plate spacing H are 0.7.Gas distributor be dicyclic gas distributor, the dicyclic gas distributor outer tube The ratio between diameter a and tower internal diameter D are 0.5, and the ratio between interior caliber b and tower internal diameter D are 0.4, in dicyclic gas distributor center and column plate The heart overlaps.
By taking ester-interchange method butyl acetate reactive distillation processes occur for methyl acetate and n-butanol as an example, as shown in Figure 3. Specific implementation process is as follows:10 blocks of column plates, pattern such as Fig. 2, tower internal diameter 200mm are installed in catalytic rectifying tower (1).Each layer tower Transesterification is filled on plate and dissipates heap granular pattern catalyst.N-butanol feeds (101) into the 2nd block of column plate of catalytic rectifying tower (1), vinegar Sour methyl esters feeds (102) into the 10th block of column plate of catalytic rectifying tower (1).Methyl acetate and n-butanol counter current contacting, and occur anti- It should be with detaching.Overhead vapours (103) main component is methyl acetate and methanol, is condensed into condenser (2), lime set (105) into return tank (3), return tank liquid phase discharging (106) passes through reflux pump (5) partial reflux (107) to catalytic rectifying tower (1), into later separation workshop section, the methyl acetate after separation is recycled to catalytic rectifying tower (1) into traveling for part extraction (110) One step ester exchange reaction.Catalytic rectifying tower (1) tower reactor be equipped with reboiler provide heat source, tower reactor main component for n-butyl acetate with Later separation and refinement are gone in n-butanol, tower reactor extraction (104), to obtain n-butyl acetate product, while the positive fourth recycled Alcohol is recycled to catalytic rectifying tower (1) and further ester exchange reaction occurs.
Using the novel major axis magnetic force pump type reactor of the present invention as catalytic distillation device, as methyl acetate and n-butanol Transesterification catalytic rectifying tower (1).Tower top operation temperature is 75 DEG C, and tower top operating pressure is 0.12MPa (A).N-butanol feeds (1) (2) molar ratio=2 are fed with methyl acetate:1, mass flow is respectively:75kg/h, kg/h, reflux ratio 12 carry out continuous Experiment, during stable operation, methyl acetate conversion per pass is up to 59.5%.
【Embodiment 5】
According to condition described in embodiment 1 and step, adjacent two pieces of column plate spacing are H, and tower internal diameter is D, H 600mm;Gas Body distributor outer tube opening diameter is 15mm, and inner tube opening diameter is 10mm, is equidistantly uniformly distributed between trepanning;The riser The ratio between diameter c and tower internal diameter D are 0.2, and riser import center and column plate centre distance are 0.3D, the descending liquid pipe diameter d with The ratio between tower internal diameter D is 0.1, and the downspout center line is 0.4D, the downspout height h and adjacent two away from column plate centre distance The ratio between block column plate spacing H is 0.9.Gas distributor be dicyclic gas distributor, the dicyclic gas distributor outer tube diameter a It is 0.7 with the ratio between tower internal diameter D, the ratio between interior caliber b and tower internal diameter D are 0.6, and dicyclic gas distributor center is weighed with column plate center It closes.
By taking ester-interchange method butyl acetate reactive distillation processes occur for methyl acetate and n-butanol as an example, as shown in Figure 3. Specific implementation process is as follows:10 blocks of column plates, pattern such as Fig. 2, tower internal diameter 200mm are installed in catalytic rectifying tower (1).Each layer tower Transesterification is filled on plate and dissipates heap granular pattern catalyst.N-butanol feeds (101) into the 2nd block of column plate of catalytic rectifying tower (1), vinegar Sour methyl esters feeds (102) into the 10th block of column plate of catalytic rectifying tower (1).Methyl acetate and n-butanol counter current contacting, and occur anti- It should be with detaching.Overhead vapours (103) main component is methyl acetate and methanol, is condensed into condenser (2), lime set (105) into return tank (3), return tank liquid phase discharging (106) passes through reflux pump (5) partial reflux (107) to catalytic rectifying tower (1), into later separation workshop section, the methyl acetate after separation is recycled to catalytic rectifying tower (1) into traveling for part extraction (110) One step ester exchange reaction.Catalytic rectifying tower (1) tower reactor be equipped with reboiler provide heat source, tower reactor main component for n-butyl acetate with Later separation and refinement are gone in n-butanol, tower reactor extraction (104), to obtain n-butyl acetate product, while the positive fourth recycled Alcohol is recycled to catalytic rectifying tower (1) and further ester exchange reaction occurs.
Using the novel major axis magnetic force pump type reactor of the present invention as catalytic distillation device, as methyl acetate and n-butanol Transesterification catalytic rectifying tower (1).Tower top operation temperature is 75 DEG C, and tower top operating pressure is 0.12MPa (A).N-butanol feeds (1) (2) molar ratio=2 are fed with methyl acetate:1, mass flow is respectively:75kg/h, 38.3kg/h, reflux ratio 12 carry out Continuous experiment, during stable operation, methyl acetate conversion per pass is up to 60.0%.
【Embodiment 6】
According to condition described in embodiment 1 and step, adjacent two pieces of column plate spacing are H, and tower internal diameter is D, H 700mm;Gas Body distributor outer tube opening diameter is 25mm, and inner tube opening diameter is 20mm, is equidistantly uniformly distributed between trepanning;The riser The ratio between diameter c and tower internal diameter D are 0.25, and riser import center and column plate centre distance are 0.2D, the descending liquid pipe diameter d with The ratio between tower internal diameter D be 0.1, the downspout center line away from column plate centre distance be 0.45D, the downspout height h with it is adjacent The ratio between two pieces of column plate spacing H are 0.9.Gas distributor be dicyclic gas distributor, the dicyclic gas distributor outer tube The ratio between diameter a and tower internal diameter D are 0.8, and the ratio between interior caliber b and tower internal diameter D are 0.7, in dicyclic gas distributor center and column plate The heart overlaps.
By taking ester-interchange method butyl acetate reactive distillation processes occur for methyl acetate and n-butanol as an example, as shown in Figure 3. Specific implementation process is as follows:10 blocks of column plates, pattern such as Fig. 2, tower internal diameter 200mm are installed in catalytic rectifying tower (1).Each layer tower Transesterification is filled on plate and dissipates heap granular pattern catalyst.N-butanol feeds (101) into the 2nd block of column plate of catalytic rectifying tower (1), vinegar Sour methyl esters feeds (102) into the 10th block of column plate of catalytic rectifying tower (1).Methyl acetate and n-butanol counter current contacting, and occur anti- It should be with detaching.Overhead vapours (103) main component is methyl acetate and methanol, is condensed into condenser (2), lime set (105) into return tank (3), return tank liquid phase discharging (106) passes through reflux pump (5) partial reflux (107) to catalytic rectifying tower (1), into later separation workshop section, the methyl acetate after separation is recycled to catalytic rectifying tower (1) into traveling for part extraction (110) One step ester exchange reaction.Catalytic rectifying tower (1) tower reactor be equipped with reboiler provide heat source, tower reactor main component for n-butyl acetate with Later separation and refinement are gone in n-butanol, tower reactor extraction (104), to obtain n-butyl acetate product, while the positive fourth recycled Alcohol is recycled to catalytic rectifying tower (1) and further ester exchange reaction occurs.
Using the novel major axis magnetic force pump type reactor of the present invention as catalytic distillation device, as methyl acetate and n-butanol Transesterification catalytic rectifying tower (1).Tower top operation temperature is 75 DEG C, and tower top operating pressure is 0.12MPa (A).N-butanol feeds (1) (2) molar ratio=2 are fed with methyl acetate:1, mass flow is respectively:75kg/h, 38.3kg/h, reflux ratio 12 carry out Continuous experiment, during stable operation, methyl acetate conversion per pass is up to 58.8%.
【Comparative example】
Methyl acetate and n-butanol enter at the top and bottom of catalytic reaction zone respectively in patent CN101219950A In catalytic rectifying tower, the two molar ratio be 1, reaction temperature be 60 DEG C, with reflux ratio 15 it is stable after, methyl acetate conversion ratio It is 58.4%.Catalytic rectifying tower catalyst is positioned in the form of catalyst packet in reaction liquid phase, difficulty is replaced, to the catalyst longevity Life requirement is high, and attainable methyl acetate conversion per pass is less than the embodiment of invention.

Claims (7)

1. a kind of novel major axis magnetic force pump type reactor, reactor is interior to be run through by 1~2 root long axis, and long axis is wrapped up by long casing, interior Portion installs bearing additional, makes axis, bearing and the medium in outside completely isolated, utilizes blade of the principle of magnetic drive pump by immersion in the medium It is coupled with axis, realizes the effect of stirring, every layer of column plate arrangement riser, riser air inlet are located at reactor long axis in reactor Side, and gas distributor is connected on riser top, gas distributor center is fallen on long axis, the gas phase from descending trays It is uniformly sprayed into the liquid-solid mixture on column plate by gas distributor, every layer of column plate is equipped with liquid phase disengaging facility, in column plate Both sides set liquid phase feeding mouth and liquid-phase outlet respectively, and column plate liquid phase enters descending trays outside tower or drop is set on column plate Liquid pipe, liquid phase flows to descending trays by upper strata column plate in tower;Solid particle or particulate catalyst are placed on every layer of column plate, Be equipped with catalyst loading and unloading mouth on every layer of column plate of reactor, can under the conditions of not parking more catalyst changeout;Wherein, adjacent two pieces of towers Plate spacing is H, and tower internal diameter is D, H ranging from 300~700mm;Gas distributor outer tube opening diameter ranging from 2~25mm, it is interior Pipe opening diameter ranging from 1~20mm, is equidistantly uniformly distributed between trepanning;The ratio between the draft tube diameter c and tower internal diameter D range It is 0.05~0.25, riser import center and column plate centre distance ranging from 0.1~0.3D, the descending liquid pipe diameter d and tower The ratio between internal diameter D ranging from 0.08~0.25, the downspout center line is away from column plate centre distance ranging from 0.20~0.45D, institute Tower tray liquid level must be stretched into hereinafter, downspout height h and adjacent two pieces of column plate spacing H ranging from 0.4~0.9 by stating downspout.
2. novel major axis magnetic force pump type reactor according to claim 1, it is characterised in that liquid-phase outlet or downcomer inlet Place is furnished with strainer, prevents catalyst from entering descending trays.
3. novel major axis magnetic force pump type reactor according to claim 1, it is characterised in that the gas distributor is ring type Gas distributor.
4. novel major axis magnetic force pump type reactor according to claim 3, it is characterised in that gas distributor is dicyclic gas Body distributor, the ratio between the dicyclic gas distributor outer tube diameter a and tower internal diameter D are 0.3~0.8, interior caliber b and tower internal diameter D The ratio between for 0.2~0.7, dicyclic gas distributor center is overlapped with column plate center.
5. novel major axis magnetic force pump type reactor according to claim 4, it is characterised in that adjacent two pieces of column plate spacing are H, Tower internal diameter is D, H ranging from 400~600mm;Gas distributor outer tube opening diameter ranging from 5~20mm, inner tube opening diameter Ranging from 5~15mm is equidistantly uniformly distributed between trepanning;The ratio between the draft tube diameter c and tower internal diameter D ranging from 0.1~ 0.15;Riser import center and column plate centre distance ranging from 0.1~0.2D;The ratio between the descending liquid pipe diameter d and tower internal diameter D Ranging from 0.1~0.15;The downspout center line is away from column plate centre distance ranging from 0.3~0.4D;The downspout height h With the ratio between adjacent two pieces of column plate spacing H ranging from 0.6~0.8.
6. novel major axis magnetic force pump type reactor according to claim 1, it is characterised in that magnetic force pump type is equipped in reactor Blender.
7. novel major axis magnetic force pump type reactor according to claim 1, it is characterised in that medium is gas-liquid-solid three-phase.
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CN110526383A (en) * 2019-08-07 2019-12-03 铜仁学院 A kind of water process ozone Oxidation Treatment device

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