CN206285877U - A kind of reaction unit of synthesizing amide - Google Patents
A kind of reaction unit of synthesizing amide Download PDFInfo
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- CN206285877U CN206285877U CN201621348070.7U CN201621348070U CN206285877U CN 206285877 U CN206285877 U CN 206285877U CN 201621348070 U CN201621348070 U CN 201621348070U CN 206285877 U CN206285877 U CN 206285877U
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Abstract
The utility model is related to a kind of reaction unit of synthesizing amide.The utility model provides a kind of reaction unit of synthesizing amide, including multiple tubular reactor, chucks for the tubular reactor to be heated or cooled connected;The tubular reactor is built with filler;The draw ratio of the tubular reactor is 20:1~1000:1.The chemical storage amount in limited workshop can be reduced using reaction unit synthesizing amide of the present utility model, it is ensured that production safety;Additionally, using reaction unit of the present utility model, it is possible to achieve the small continuous production few with reaction volume in the unit interval of conversion zone, thus easy control of reaction system is so as to accomplish scale production;In addition, synthetic reaction classification is carried out, saving energy consumption adjustable per order reaction temperature shortens the reaction time, improve production efficiency.The reaction unit that the utility model is provided, is especially suitable for the reaction of synthesizing amide under solvent free conditions.
Description
Technical field
The utility model is related to a kind of reaction unit of synthesizing amide.
Background technology
Acid amides is industrially widely used usually as solvent and synthetic intermediate, for example DMF
And DMAC N,N' dimethyl acetamide (DMAC) is all good organic solvent (DMF).Acid amides generally passes through acid and amine, or by ester
Reaction between amine is obtained, and the reaction unit for being usually used in acid amides synthesis is mostly the barrel type reactor of low ratio of height to diameter, mostly
Batch (-type) tank reactor.Because tank reactor generally has larger capacity, it is therefore desirable to stored in workshop space
Chemical volume it is big;Additionally, in the chemical reaction of synthesizing amide, the reactant and/or solvent for using belong to hazardous chemical, because
The storage capacity of this hazardous chemical in workshop is big, easily produces safety problem.In addition, the reaction of some synthesizing amides, can be with
Carry out under solvent free conditions;However, in tank reactor, when solvent diluting reaction thing is not used, reactant is dense
Degree is very big, and heat release or endothermic effect are also very big during reaction, and different zones temperature is different in kettle, are easily caused reaction uneven;
And different zones reaction is asynchronous, fuel factor difference can reduce reaction temperature, extension reaction time, cause production efficiency to drop
It is low.
The content of the invention
In order to solve the above technical problems, the utility model provides a kind of reaction unit of synthesizing amide, including multiple series connection
Tubular reactor, be coated on outside tubular reactor and be used to that the chuck of the tubular reactor to be heated or cooled;The tubular type is anti-
Device is answered built with filler;The draw ratio of the tubular reactor is 20:1~1000:1.
The chemical storage amount in limited workshop can be reduced using reaction unit synthesizing amide of the present utility model,
Ensure production safety.Additionally, using reaction unit of the present utility model, can be conversion zone be small and reactant in the unit interval
Continuously produced under conditions of amount is few, thus easy control of reaction system is so as to accomplish scale production.In addition, synthetic reaction classification is carried out,
Adjustable, the saving energy consumption per order reaction temperature, shortens the reaction time, improve production efficiency.The reaction unit that the utility model is provided,
It is especially suitable for the reaction of synthesizing amide under solvent free conditions.
The utility model makes raw material that flow-disturbing is formed in flowing by the combination of the caliber of tubular reactor when filler,
Mixed effect between increase reaction mass, mass transfer enhancement heat-transfer effect.The utility model changes tubular reactor by filler
Caliber and pipe inner structure, by the caliber of tubular reactor, when the best combination of filler strengthens raw material and mixes and mass-and heat-transfer
Effect.
The preferred stainless steel of material of the filler loaded in tubular reactor is improving corrosion resistance;The utility model each fill out
The volume of material includes the solid volume of each filler and the volume of filler itself hole.The total volume of filler in the utility model
(solid volume of i.e. all fillers with itself pore volume sum) account for tubular reactor volume of the present invention 90% and
More than;Preferably, the utility model filler fills up described whole tubular reactor.The utility model is by anti-to each tubular type
Answer device that chuck is set, so as to control the reaction temperature of each tubular reactor by the way that chuck is heated or cooled.Additionally, this practicality
It is new to be more accurately controlled the temperature of charge and proportioning of reaction by the way that tubular reactor is connected.And simultaneously joint conference can not keep away
The generation reactant ratio exempted from is poor, and causes sectional temperature-controlled nonsensical.
Generally, the filler in tubular reactor is used as catalyst bed, and reaction mass is reacted by catalyst, filler
It is exactly beds.And the acid amides reaction in the utility model can be carried out under the reaction condition participated in without catalyst.
The main purpose that filler is disposed in the utility model tubular reactor is the interior knot of caliber and pipe by changing tubular reactor
Structure, the flowing to raw material forms flow-disturbing, increases the mixed effect between reaction mass, and mass transfer enhancement heat-transfer effect.As one
Implementation method is planted, described filler is at least one of Raschig ring, western tower ring and Pall ring.When filler of the present utility model is western to draw
When at least one of ring, western tower ring and Pall ring, can further change the caliber and pipe inner structure of tubular reactor, to original
The flowing of material forms more preferable flow-disturbing, the further mixed effect between increase reaction mass, and mass transfer enhancement heat-transfer effect.Make
It is a kind of implementation method, the single entity volume of the Raschig ring, western tower ring and Pall ring is identical in tubular reactor;The drawing
The quantity ratio of western ring, western tower ring and Pall ring is (0~50):(50~100):(0~50).The utility model is different by controlling
Species filler quantitative proportion can reach more excellent caliber and pipe inner structure;And can be with the real reaction space in control pipe
(real reaction space includes hole, the space between filler and tube wall and between filler and filler of filler itself).Work as tubular type
The quantity ratio of the equal Raschig ring of single entity volume, western tower ring and Pall ring is (20~70) in reactor:(50~100):
When (0~20), the reaction compartment for reaching is the 65~95% of the tubular reactor volume.Further, when single entity body
The quantity ratio of product equal Raschig ring, western tower ring and Pall ring is (40~70):(60~100):When (0~10), what is reached is anti-
Answer that space is the tubular reactor volume 75~95%.Further, when the equal Raschig ring of single entity volume, west
The quantity ratio of tower ring and Pall ring is (50~80):(70~100):When (0~5), the reaction compartment for reaching is that the tubular type is anti-
Answer the 12~95% of body product.While above-mentioned reaction compartment can make reactant be fully contacted and react, the effect of reaction is improved
Rate.The utility model Fillers selection according to the characteristics of reaction raw materials and appropriate, can to a certain extent shorten tubular type anti-
Answer the total length of device.When described filler is western tower ring, the mass transfer residence time can be increased, make reaction mass in western tower ring filler table
Face mass transfer fully, is well mixed, to improve conversion ratio.If the space that reactant is reacted in tubular reactor is very few,
Slow down the flowing velocity of reaction mass, extend the time of contact of reaction mass, reduce reaction rate;If reactant is in pipe reaction
The space reacted in device is excessive, then mass-and heat-transfer is insufficient, reduces reaction conversion ratio and yield.Therefore, the utility model
The reaction compartment combined to form by filler and caliber, can further improve the reaction rate of acid amides, and then improve conversion ratio
And yield.The utility model each tubular reactor, the body proportioning of filler can be with identical, it is also possible to differs;Caliber can also
It is identical, can differ.
Used as a kind of implementation method, the draw ratio of the tubular reactor is 50:1~500:1.Preferably, the tubular type
The draw ratio of reactor is 100:1~200:1.Used as a kind of implementation method, the draw ratio of the tubular reactor is 20:1~
50:1.Used as a kind of implementation method, the draw ratio of the tubular reactor is 700:1~1000:1.The utility model classification control
Temperature, it is safe and efficient.According to the function of every one-level pipe, the draw ratio of pipe is adjusted, such as 3 or 4 tubular reactors are composed in series
Reaction unit, feed pipe is referred to as the first stage reactor, and by that analogy, the first stage reactor (i.e. feed pipe) is with mixed reactant
For the purpose of material, draw ratio is suitably reduced, and it is 50~100 that can select draw ratio:1;Second stage reactor, as key reaction
Institute, draw ratio suitably increases, and it is 200~300 that can select draw ratio:1;Third level reactor is (if desired, it is also possible to save
But), draw ratio is suitably reduced, and it is 100~200 that can select draw ratio:1;Fourth stage reactor (discharging opening), rises and cools
Effect, draw ratio is smaller, and it is 50~100 that can select draw ratio:1.
The utility model does not limit the number of tubular reactor, can carry out according to actual needs, but combine cost etc. because
Plain preferably tubular reactor number is 3~6.The further preferred tubular reactor number is 3 or 4.
The utility model multiple reactor series connection, each temperature of reactor is adjustable, can be maximum according to the characteristics of reaction
Limit utilizes thermal source.In one embodiment, water flowing in the chuck of the tubular reactor of charging and the tubular reactor of discharging
Cooling.For example, the reaction unit that 3 or 4 tubular reactors are composed in series, in first order tubular reactor (feed pipe), closes
Reactant into acid amides each leads into wherein and mixes, and is reacted during being mixed due to reactant, produces fuel factor, because
, by the cooling water control temperature of reactor in chuck, suppressing reaction is carried out for this;It is serially connected with the second of first order tubular reactor
In level tubular reactor, by leading to steam or electrically heated mode heating response device in chuck, reacting fully is carried out;Concatenation
In the third level tubular reactor of second level tubular reactor (if desired, it is also possible to save), by leading to steam in chuck
Or electrically heated mode heating response device, high-temperature is further risen, make reaction complete;It is serially connected with third level tubular reactor
In afterbody tubular reactor (discharge nozzle), by the cooling water control temperature of reactor in chuck, product is lowered the temperature, prepare
Discharging.
For example, the reaction unit that 3 or 4 tubular reactors are composed in series, reaction raw materials are entered by bottom feed mouthful respectively
Enter in first tubular reactor, charging rate is controlled by measuring pump or mass flowmenter.Such as with ester and amine as reactant
The mol ratio of synthesizing amide, ester and amine is 0.5:1~1:0.5.Preferably 0.95:1~1.05:1.Further preferred 0.99:1~
1.01:1.Tandem type multi-stage tubular reactor, high conversion rate close to 100%, is particularly suitable for by equimolar than the reaction that carries out,
Because reaction raw materials less residue in the product for obtaining, therefore, it can by close to 1:1 mol ratio charging.Synthesizing amide it is anti-
Should, can carry out under solvent free conditions, solvent is not involved in reaction, saves the steps such as separation, purification, Simplified flowsheet, drop
Low cost.The reaction of the synthesizing amide that the utility model is participated in preferably without solvent, reaction raw materials are being mounted with the tubular type of filler
It is well mixed in reactor, water flowing regulation temperature in first order tubular reactor chuck, below 80 DEG C of reactor temperature of control.
Preliminary well mixed reaction raw materials enter participation reaction in the tubular reactor of the second level, by the temperature of thermal medium in chuck
Or electrically heated mode heating response device, 80~150 DEG C of controlling reaction temperature, preferably 100~130 DEG C;To ensure that reaction is filled
Point, can select to enter third level tubular reactor, by controlling the temperature of thermal medium or electrically heated mode in chuck
Heating response device, preferably 150~250 DEG C of controlling reaction temperature, 150~200 DEG C.If reaction rate is fast, reaction is easily carried out.
Fully after reaction, into fourth stage reactor, water flowing regulation temperature in reactor jacket, 100 DEG C of reactor temperature of control with
Under, preferably less than 80 DEG C, then discharged from reactor head, into products pot storage.
Used as a kind of implementation method, when the caliber of tubular reactor is 2~20mm, the tubular reactor is by upper and lower two
Duan Guanzi connection compositions;When the caliber of tubular reactor is 20~10000mm, the tubular reactor is by section of a pipe group
Into.It is preferred that tubular reactor is directly made up of section of a pipe, pipe end is connected with flange.The tubular reactor small for caliber, it is excellent
Select each tubular reactor to be made up of two sections pipe, connected with fastener between two sections of pipes, connect appropriate after loading filler,
Because filler diameter is bigger than the diameter of feed pipe and discharge nozzle, filler is stayed in pipe.The tubular reactor big for caliber, it is each
Level tubular reactor uses section of a pipe, and pipe end is coupled using flange, to facilitate the placement of filler.After raw material enters in pipe, lead to
The flow-disturbing effect for crossing filler makes liquid material make irregular movement, in addition to the flowing for being parallel to tubular reactor, also hangs down
The straight flowing in flow tube axis direction is produced, so that mass transfer enhancement conducts heat.
As a kind of implementation method, when the caliber of tubular reactor is 2~20mm, the volume of single filler (including list
Itself solid volume of individual filler and pore volume) preferably 1~5mm3;It is single when the caliber of tubular reactor is 20~10000mm
The volume of individual filler is preferably 5~100mm3;When the caliber of tubular reactor is 100~500mm, the volume of single filler is excellent
Elect 10~50mm as3.At least one of the above-mentioned preferred Raschig ring of filler, western tower ring and Pall ring;And single entity volume is equal
Raschig ring, western tower ring and Pall ring quantity ratio be (0~50):(50~100):(0~50).Further, single entity
The quantity ratio of the equal Raschig ring of volume, western tower ring and Pall ring is (20~70):(50~100):(0~20).Further,
The quantity ratio of the equal Raschig ring of single entity volume, western tower ring and Pall ring is (40~70):(60~100):(0~10).
Further, the quantity ratio of the equal Raschig ring of single entity volume, western tower ring and Pall ring is (50~80):(70~100):
(0~5).Further, preferably western tower ring.
In addition to tubular reactor, reaction unit also includes head tank, solvent tank, products pot, circulating heat exchange medium groove, meter
Amount pump, flowmeter, cutting ferrule pipe and valve etc., are not limited to above-mentioned auxiliary equipment, instrument, can increase and decrease according to actual needs.
Brief description of the drawings
Fig. 1:The utility model includes 4 reaction units of tubular reactor;
Fig. 2:The tubular reactor structural representation of two sections pipe connection in the utility model;
In figure, 1- fillers;2- tubular reactors;3- discharging openings;4- chucks;5- fasteners;6- charging apertures.
Specific embodiment
Following specific embodiment is described in detail to the utility model, but the utility model is not restricted to
Following examples.
Embodiment 1:
A kind of reaction unit of synthesizing amide, including head tank (storage reactant), solvent tank (storage methyl alcohol or ethanol),
Products pot, the tubular reactor 2 of series connection and circulating heat exchange medium groove, measuring pump, flowmeter, cutting ferrule pipe, valve etc. are some.
Feedstock direction as shown in Figure 1 is sequentially connected in series 4 tubular reactors 2 to discharging direction, and is named as successively since charging aperture
First order tubular reactor, second level tubular reactor, third level tubular reactor and fourth stage tubular reactor (discharging opening pair
The tubular reactor answered).Each outside of tubular reactor 2 is coated with chuck 4.Each tubular reactor is described built with filler 1
Filler is western tower ring.So that ester and amine are reactant synthesizing amide as an example, reaction raw materials enter tubular type by bottom feed mouthful 6 respectively
In reactor 2 (draw ratio 125), and charging rate controlled by measuring pump or mass flowmenter respectively, ester and amine it is logical
It is 0.99 to enter amount ratio (mol ratio):1.02.Reaction raw materials mixing, reactor jacket in first order tubular reactor (feed pipe)
Interior logical running water regulation temperature, below 60 DEG C of reactor temperature of control.Well mixed reaction compound is from first order tubular type
The discharging opening 3 of reactor enters second level tubular reactor (draw ratio 100) and participates in reaction after being input into.By jacket steam plus
Thermal reactor, 80~100 DEG C of controlling reaction temperature, to ensure that reaction is abundant, into third level tubular reactor (draw ratio 50),
By steam heating response device, about 130 DEG C of controlling reaction temperature.Then, into fourth stage tubular reactor (draw ratio 80), instead
Water flowing regulation temperature in device chuck is answered, below 100 DEG C of reactor temperature of control, is then discharged from reactor head, into product
Product tank is stored.
Embodiment 2:
A kind of reaction unit of synthesizing amide, including head tank, the tubular reactor 2 and circulating heat exchange medium of series connection
Groove, measuring pump, flowmeter, cutting ferrule pipe, valve etc. are some.By feedstock direction 3 tubular reactors are sequentially connected in series to discharging direction
2, and it is named as first order tubular reactor, second level tubular reactor and third level tubular reactor successively since charging aperture
(the corresponding tubular reactor of discharging opening).Each outside of tubular reactor 2 is coated with chuck 4.Each tubular reactor built with
Filler 1, described filler is Raschig ring, western tower ring and Pall ring.The quantity ratio of the Raschig ring, western tower ring and Pall ring is 20:
70:10.So that ester and amine are reactant synthesizing amide as an example, reaction raw materials enter first order tubular type by bottom feed mouthful 6 respectively
In reactor (draw ratio 125), and charging rate controlled by measuring pump or mass flowmenter respectively, ester and amine are passed through
Amount is 0.8 than (mol ratio):1.Reaction raw materials mix in first order tubular reactor, and running water regulation is led in reactor jacket
Temperature, below 80 DEG C of reactor temperature of control.Well mixed reaction compound enters second level tubular reactor (draw ratio
125) reaction is participated in.By jacket steam heating response device, 150 DEG C of controlling reaction temperature.Then, it is anti-into third level tubular type
Device (draw ratio 125) is answered, water flowing regulation temperature in reactor jacket, below 80 DEG C of reactor temperature of control, then from reaction
Device top discharge, into products pot storage.
Embodiment 3:
A kind of reaction unit of synthesizing amide, including head tank, the tubular reactor 2 and circulating heat exchange medium of series connection
Groove, measuring pump, flowmeter, cutting ferrule pipe, valve etc. are some.By feedstock direction 3 tubular reactors are sequentially connected in series to discharging direction
2, and it is named as first order tubular reactor, second level tubular reactor and third level tubular reactor successively since charging aperture
(the corresponding tubular reactor of discharging opening).Each tubular reactor 2 is made up of two sections of pipes, and two sections of pipes are connected by fastener 5,
Each outside of tubular reactor 2 is coated with chuck 4.Built with filler 1, described filler is Raschig ring, west to each tubular reactor
Tower ring and Pall ring.The quantity ratio of the Raschig ring, western tower ring and Pall ring is 30:65:5.It is reactant synthesis with ester and amine
As a example by acid amides, reaction raw materials are entered in first order tubular reactor (draw ratio 50) by bottom feed mouthful respectively, and respectively
By measuring pump or mass flowmenter control charging rate, intake ratio (mol ratio) of ester and amine is 1.01:1.Reaction is former
Material mixes in first order tubular reactor, and running water regulation temperature is led in reactor jacket, controls 80 DEG C of reactor temperature
Below.Well mixed reaction compound enters second level tubular reactor (draw ratio 150) and participates in reaction.By electrical heating side
Formula heating response device, 120~130 DEG C of controlling reaction temperature.Then, into third level tubular reactor (draw ratio 30), reaction
Water flowing regulation temperature in device chuck, below 80 DEG C of reactor temperature of control, then discharges, into products pot from reactor head
Storage.
Claims (12)
1. a kind of reaction unit of synthesizing amide, it is characterised in that:Including multiple tubular reactors connected, it is coated on the pipe
It is used to be heated or cooled the chuck of the tubular reactor outside formula reactor;The tubular reactor is built with filler;The pipe
The draw ratio of formula reactor is 20:1~1000:1.
2. reaction unit as claimed in claim 1, it is characterised in that:Described filler is in Raschig ring, western tower ring and Pall ring
It is at least one.
3. reaction unit as claimed in claim 2, it is characterised in that:The equal Raschig ring of single entity volume, western tower ring and
The quantity ratio of Pall ring is (0~50):(50~100):(0~50).
4. reaction unit as claimed in claim 2, it is characterised in that:The equal Raschig ring of single entity volume, western tower ring and
The quantity ratio of Pall ring is (20~70):(50~100):(0~20).
5. reaction unit as claimed in claim 4, it is characterised in that:The equal Raschig ring of single entity volume, western tower ring and
The quantity ratio of Pall ring is (40~70):(60~100):(0~10).
6. reaction unit as claimed in claim 2, it is characterised in that:The equal Raschig ring of single entity volume, western tower ring and
The quantity ratio of Pall ring is (50~80):(70~100):(0~5).
7. reaction unit as claimed in claim 2, it is characterised in that:Described filler is western tower ring.
8. reaction unit as claimed in claim 1, it is characterised in that:The draw ratio of the tubular reactor is 50:1~500:
1。
9. reaction unit as claimed in claim 8, it is characterised in that:The draw ratio of the tubular reactor is 100:1~
200:1。
10. reaction unit as claimed in claim 1, it is characterised in that:The tubular reactor is 3~6.
11. reaction units as claimed in claim 1, it is characterised in that:The tubular reactor of charging and the pipe reaction of discharging
Water flowing cooling in the chuck of device.
12. reaction units as claimed in claim 1, it is characterised in that:The caliber of the tubular reactor is 2~20mm and institute
Tubular reactor is stated to be made up of the connection of two sections pipe;Or the caliber of the tubular reactor is 20~10000mm and described
Tubular reactor is made up of section of a pipe.
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CN107670594A (en) * | 2017-11-10 | 2018-02-09 | 大丰鑫源达化工有限公司 | A kind of device of continous way speed up gas and liquid reaction |
CN108079932A (en) * | 2018-02-01 | 2018-05-29 | 贵州道元生物技术有限公司 | The continuous flow deferent Dow Chemical reactor of fast assembling-disassembling |
CN109663546A (en) * | 2019-02-21 | 2019-04-23 | 南京科技职业学院 | A kind of antifebrin synthesis special purpose reactor |
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CN110394143A (en) * | 2019-08-21 | 2019-11-01 | 兖州煤业股份有限公司 | A kind of coal resolution tubular type reaction unit |
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CN107670594A (en) * | 2017-11-10 | 2018-02-09 | 大丰鑫源达化工有限公司 | A kind of device of continous way speed up gas and liquid reaction |
CN108079932A (en) * | 2018-02-01 | 2018-05-29 | 贵州道元生物技术有限公司 | The continuous flow deferent Dow Chemical reactor of fast assembling-disassembling |
CN109663546A (en) * | 2019-02-21 | 2019-04-23 | 南京科技职业学院 | A kind of antifebrin synthesis special purpose reactor |
CN109663546B (en) * | 2019-02-21 | 2022-09-06 | 南京科技职业学院 | Special reactor for synthesizing acetanilide |
CN110252236A (en) * | 2019-07-08 | 2019-09-20 | 湖北仙粼化工有限公司 | A kind of diethanol monoisopropanolamine production multiple spot mixing reactor |
CN110394143A (en) * | 2019-08-21 | 2019-11-01 | 兖州煤业股份有限公司 | A kind of coal resolution tubular type reaction unit |
CN110394143B (en) * | 2019-08-21 | 2024-06-07 | 兖矿能源集团股份有限公司 | Tubular reaction device is cleared up to coal |
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CN113185561A (en) * | 2021-04-24 | 2021-07-30 | 无锡济煜山禾药业股份有限公司 | Method for obtaining 1-N-ethyl gentamicin C1a by pipeline reaction hydrolysis |
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