CN209362482U - Aromatic carboxy acid compound's nitration reaction equipment therefor - Google Patents

Aromatic carboxy acid compound's nitration reaction equipment therefor Download PDF

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Publication number
CN209362482U
CN209362482U CN201821963786.7U CN201821963786U CN209362482U CN 209362482 U CN209362482 U CN 209362482U CN 201821963786 U CN201821963786 U CN 201821963786U CN 209362482 U CN209362482 U CN 209362482U
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mixed cell
tubular reactor
mixing tube
overhead gage
import
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CN201821963786.7U
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Chinese (zh)
Inventor
邢政国
丁玉
戴明松
陈晨
杨国泉
冯柏成
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Qingdao Tamar New Mstar Technology Ltd
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Qingdao Tamar New Mstar Technology Ltd
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Abstract

The utility model belongs to organic compound reaction equipment therefor field, and in particular to a kind of nitration reaction equipment therefor of aromatic carboxy acid compound.The device includes mixer, tubular reactor, glass reaction kettle;Mixer includes mixing tube, and there is nitration mixture outlet in the rear end of mixing tube;Nitration mixture outlet is connected with the import of the left upper end of tubular reactor;The discharge port of tubular reactor right end is connected with the import of glass reaction kettle, and the right end discharge outlet of tubular reactor has valve.By using the device of the utility model, in one end of mixer, two strands of material inlets are set, two strands of materials carry out strong mechanical stirring in tubular reactor after being sufficiently mixed by mixer make organic phase solid be dispersed to completion reaction in sour phase, reduce the dosage of the concentrated sulfuric acid, and heat-transfer effect is good when reacting, reaction speed is improved, the generation of side reaction is reduced, while reducing the risk of reaction.

Description

Aromatic carboxy acid compound's nitration reaction equipment therefor
Technical field
The utility model belongs to organic compound reaction equipment therefor field, and in particular to a kind of aromatic carboxy acid compound Nitration reaction equipment therefor.
Background technique
Most important nitration reaction is the nitrification of aromatic hydrocarbons in organic chemistry, and the most important effect of nitro is introduced on aromatic ring It is and then to prepare the compounds such as phenol, fluoride as preparing an important channel of amino-compound.
Traditional nitration method mainly include the following types:
(1) dust technology nitrification is generally used for the nitrification of the aromatic compound containing strong first kind positioning base, and reaction exists It is carried out in stainless steel or enamel equipment, nitric acid about excessive 10 ~ 65%.
(2) concentrated nitric acid nitrifies this nitrification and often must try to utilize with excessively many nitric acid again, excessive nitric acid Or recycling, thus it is restricted its practical application.
(3) the homogeneous nitrification in concentrated sulfuric acid medium is when being at the reaction temperatures solid by itrated compound or nitration product, often It will be often dissolved in by itrated compound in a large amount of concentrated sulfuric acids, sulfuric acid is then added and the mixture of nitric acid is nitrified.This method is only It needs using excessive seldom nitric acid, general yield is higher, the disadvantage is that sulfuric acid dosage is big.
(4) heterogeneous mixed acid nitrification is usually used when being all at the reaction temperatures liquid by itrated compound or nitration product The method of heterogeneous mixed acid nitrification makes organic phase be dispersed in sour phase and complete nitration reaction by strong stirring.
(5) the advantages of nitrifying this method in organic solvent is usually can change obtained using different solvents The ratio of nitro isomerized products avoids making solvent using a large amount of sulfuric acid, and uses the nitric acid close to theoretical amount.It is common organic Solvent has acetic acid, acetic anhydride, dichloroethanes etc..
Since aromatic carboxylic-acid compound has passivation group's carboxyl on phenyl ring, it is difficult to be nitrified so comparing, tradition Technique be to be raised to reaction temperature nitration mixture is added dropwise again after concentrated sulfuric acid dissolution aromatic carboxylic acids, need after reaction dilute with a large amount of water The shortcomings that releasing concentrated sulfuric acid material can just be precipitated, this technique is to generate a large amount of spent acid, is produced simultaneously as certain isomerization can be generated Object and more nitro products, reduce yield.And traditional tank reactor, when being reacted, substrate is due to a large amount of sulfuric acid Presence, viscosity is very big, and mobility is poor, leverage the heat-transfer effect of nitration reaction, simultaneously because nitration reaction be put Thermal response, temperature is higher, and the speed of nitration reaction is faster, and the heat of releasing is more, more easily causes temperature control and explodes.
Organic solvent nitration method reported in the literature is mostly to carry out mixed acid nitrification again after dissolving raw material with solvent, and the method is anti- It also needs to carry out cumbersome post-processing after answering, equipment and energy consumption are higher.
Consersion unit above method defect and compatible with new method can be overcome by inventing one kind at present.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of nitration reactions suitable for aromatic carboxy acid compound Equipment therefor, aromatic carboxylic acid chemical combination carry out nitration reaction by the device, and purity and yield are all higher.
Its specific structure of the device of the utility model is as follows:
Aromatic carboxy acid compound's nitration reaction equipment therefor, the device include mixer and the pipe that is connected with mixer Formula reactor further includes glass reaction kettle;
Mixer includes mixing tube, has the first import in the left end of mixing tube, and the upper top of left end has the second import, mixing There is nitration mixture outlet in the rear end of pipe, there is multiple mixed cells, the import of nitration mixture outlet and the left upper end of tubular reactor in mixing tube It is connected;
There is agitating device in the left end of tubular reactor, and agitating device includes agitating shaft and blade, and agitating shaft passes through with motor Shaft coupling is connected and its rotation is driven by motor;
There are multiple temperature sensors, multiple pressure sensors in tubular reactor;
Temperature sensor, pressure sensor are connected with display screen respectively, and display location is in the lateral wall of tubular reactor On;
The lower-left end of tubular reactor is provided with drain, is corresponding with valve at drain;
The discharge port of tubular reactor right end is connected with the import of glass reaction kettle, the right end discharge port of tubular reactor There is valve at place.
Mixing tube is double layer jacket structure.
The lower-left end of mixing tube has import to be connected with collet, and the upper right side of mixing tube has outlet to be connected with collet.
First import is connected with the first feed pipe, and the second import is connected with the second feed pipe;Have on first feed pipe First flowmeter has second flowmeter on the second feed pipe.
There are three temperature sensors, three pressure sensors in tubular reactor;Temperature sensor and pressure sensor are handed over For being intervally arranged, the spacing between adjacent temperature sensor and pressure sensor is equal.
Tubular reactor is double layer jacket structure, and there are water inlet, the upper right of tubular reactor in the lower-left end of tubular reactor There is water outlet at end.
Blade inside tubular reactor is screw type blade, centered on agitating shaft set by the agitating shaft It sets.
The structure of mixed cell is as follows: the first mixed cell of left end is located at below the first import, the first mixed cell Interior lower bottom part has magnetic rotor, and the mixing tube lower bottom part outside the first mixed cell has magnetic stirring apparatus, and the first mixed cell is right While being the second mixed cell, the second mixed cell is by positioned at the first overhead gage of its left end, the first lower baffle plate and positioned at its right end Second baffle surrounded;
First overhead gage and the first lower baffle plate shapes and sizes are identical, the first overhead gage and the upper top for mixing inside pipe wall Portion is connected, and the first lower baffle plate is connected with the lower bottom part of mixing inside pipe wall, and on the first overhead gage lower end and the second overhead gage The distance between end is equal with the first overhead gage/height of the first lower baffle plate;
Upper mesh areas and lower mesh areas, upper mesh areas account for the 1/ of second baffle area respectively for the upper and lower part of second baffle 6, lower mesh areas accounts for the 1/6 of second baffle area;
Third mixed cell is by being located at the second baffle of its left end and positioned at the third overhead gage and third lower block of its right end Plate is surrounded;
Remaining mixed cell repeats the second mixed cell and third mixed cell is alternately present.
The structure of mixed cell can also be as follows:
First mixed cell of left end is located at below the first import, and the lower bottom part in the first mixed cell has magnetic force to turn Son, the mixing tube lower bottom part outside the first mixed cell have magnetic stirring apparatus, are the second mixed cells on the right of the first mixed cell, the Two mixed cells are by being located at the first overhead gage of its left end and being surrounded positioned at the first lower baffle plate of its right end;First overhead gage and The shapes and sizes of first lower baffle plate are identical;First overhead gage is connected with the upper top of mixing inside pipe wall, the first lower block Plate is connected with the lower bottom part of mixing inside pipe wall, and the lower bottom part of the first overhead gage is located at the lower section of mixing tube cross central line, the The upper top of one lower baffle plate is located at the top of mixing tube cross central line;Third mixed cell, the 4th mixed cell ... .. N are mixed The structure that unit repeats the second mixed cell is closed, N is the positive integer greater than 4.
The distance between first overhead gage and the first lower baffle plate are at least greater than or equal to the 2/3 of the first overhead gage height.
The beneficial effects of the present invention are by using the nitration reaction institute of the aromatic carboxy acid compound of the utility model With device, two strands of material inlets are set in one end of mixer, two strands of materials be sufficiently mixed by mixer after in pipe reaction Strong mechanical stirring is carried out in device makes organic phase solid be dispersed to completion reaction in sour phase, reduces the dosage of the concentrated sulfuric acid, And heat-transfer effect is good when reacting, and improves reaction speed, reduces the generation of side reaction, while reducing the danger of reaction Property.
Detailed description of the invention
Fig. 1 is the mixer structure schematic diagram of embodiment 1;
Fig. 2 is the enlarged structure schematic diagram of the second baffle of mixer in embodiment 1;
Fig. 3 is the structural schematic diagram of the tubular reactor in embodiment 1;
Fig. 4 is the overall structure diagram of embodiment 1;
Fig. 5 is the mixer structure schematic diagram of embodiment 2;
Fig. 6 is the mixer structure schematic diagram of embodiment 3;
Fig. 7 is the mixer structure schematic diagram of embodiment 4;
In figure, 1- mixing tube, 2- second baffle, 3- magnetic stirring apparatus, 4- magnetic rotor, the first import of 101-, 102- Two imports, the first overhead gage of 201-, the first lower baffle plate of 202-, the second overhead gage of 203-, the second lower baffle plate of 204-, the upper mesh of 205- Area, mesh areas under 206-, the outlet of 207- nitration mixture, the first collet of 208-, 5- tubular reactor, the first temperature sensor of 501-, 502- first pressure sensor, 503- second temperature sensor, 504- second pressure sensor, 505- third temperature sensor, 506- third pressure sensor, 507- drain, 508- water inlet, 509- water outlet, 510- discharge port, 511- import, 512- Agitating device, 514- blade;The second collet of 515-.6- glass reaction kettle, 7- mixer.
Specific embodiment
Next with reference to the accompanying drawings and detailed description the present invention will be further explained, so as to the technology of this field Personnel know more about the present invention, but do not limit the utility model with this.
Embodiment 1
Aromatic carboxy acid compound's nitration reaction equipment therefor, the device include mixer 7 and are connected with mixer 7 Tubular reactor 5 further includes glass reaction kettle 6;
Mixer 7 includes mixing tube 1, has the first import 101 in the left end of mixing tube 1, the upper top of left end have second into Mouth 102, the rear end of mixing tube 1 have nitration mixture to export 207, there is multiple mixed cells in mixing tube 1, and nitration mixture outlet 207 is anti-with tubular type The import 511 of the left upper end of device 5 is answered to be connected;
There is agitating device 512 in the left end of tubular reactor 5, and agitating device 512 includes agitating shaft and blade 514, agitating shaft It is connected with motor by shaft coupling and its rotation is driven by motor;(above structure is conventional structure, because not marking in figure Note)
It is successively that the first temperature passes from left to right there are three temperature sensor, three pressure sensors in tubular reactor 5 Sensor 501, first pressure sensor 502, second temperature sensor 503, second pressure sensor 504, third temperature sensor 505, third pressure sensor 506;Temperature sensor and pressure sensor alternate intervals are arranged, adjacent temperature sensor and pressure Spacing between force snesor is equal.
Temperature sensor, pressure sensor are connected with display screen respectively, and display location is in the lateral wall of tubular reactor On;
The lower-left end of tubular reactor 5 is provided with drain 507, is corresponding with valve at drain 507;The effect of drain It is thoroughly to give off the material in tubular reactor 5;
The discharge port 510 of 5 right end of tubular reactor is connected with the import of glass reaction kettle 6, the right end of tubular reactor 5 There is valve at discharge port 510.
First import 101 is connected with the first feed pipe, and the second import 102 is connected with the second feed pipe;First charging Guan Shangyou first flowmeter has second flowmeter on the second feed pipe, is respectively used to metering feeding rate.
Tubular reactor 5 is double layer jacket structure, and there are water inlet 508, tubular reactor 5 in the lower-left end of tubular reactor 5 Upper right side have water outlet 509.
Blade inside tubular reactor 5 is screw type blade 514, around agitating shaft institute centered on agitating shaft Setting.
The specific structure of mixed cell is as follows:
First mixed cell of left end is located at 101 lower section of the first import, the bottom in the first mixed cell in mixing tube 1 There is magnetic rotor 4 in portion, and 1 lower bottom part of mixing tube outside the first mixed cell has a magnetic stirring apparatus 3, is the on the right of the first mixed cell Two mixed cells, the second mixed cell is by positioned at the first overhead gage 201 of its left end, the first lower baffle plate 202 and positioned at its right end Second baffle 2 surrounded;
First overhead gage 201 is identical with 202 shapes and sizes of the first lower baffle plate, the first overhead gage 3201 and mixing tube The upper top of 1 inner wall is connected, and the first lower baffle plate 202 is connected with the lower bottom part of 1 inner wall of mixing tube, and the first overhead gage 201 Lower end and the distance between the second overhead gage upper end are equal with the height of 201/ first lower baffle plate 202 of the first overhead gage;
There are upper mesh areas 205 and lower mesh areas 206 in the upper and lower part of second baffle 2 respectively, and upper mesh areas 205 accounts for second The 1/6 of 2 area of baffle, lower mesh areas 206 account for the 1/6 of 2 area of second baffle;
Third mixed cell is by being located at the second baffle 2 of its left end and positioned at the third overhead gage and third lower block of its right end Plate is surrounded;
Remaining mixed cell repeats the second mixed cell and the structure of third mixed cell is alternately present.
In order to better illustrate the utility model, the present inventor carries out in conjunction with the nitration reaction of aromatic carboxy acid compound It illustrates, the process of nitration reaction is:
The technique that aromatic carboxy acid compound nitrifies in tubular reactor, its step are as follows:
(1) sulfuric acid of the nitric acid of 864g 95% and 1728g 98% are configured to nitration mixture;
(2) 2000g parachlorobenzoic-acid and 8000g dichloroethanes are beaten, obtain pasty material;
(3) nitration mixture in (1) and the pasty material in (2) are sent into mixer, control pasty material flow velocity is 100g/ Min, nitration mixture flow velocity is 26g/min, and is kept for 20 DEG C of mixer temperature or so, and it is anti-to enter back into tubular type after mixing by mixer It answers in device and reacts, tubular reactor interior reaction temperature is maintained at 50 DEG C or so, and tubular reactor length about 2.5m, the residence time is about 15min, discharging enter 20L glass reaction kettle, improve glass reaction temperature to 55 DEG C, the reaction was continued 1h, subsequently into aging pan Detection, when HPLC detects parachlorobenzoic-acid content < 0.5%, discharging;
(4) enter centrifuge after discharging, centrifugal rotational speed 1200r/min is centrifugated solid liquid phase, and liquid phase enters separator Reuse respectively dries to obtain 2394.5g solid product, HPLC after solid is eluted with 2000ml water after isolating organic phase and sour phase The purity of testing product is 99.8%, yield 93.0%;
Gained liquid enters separator and carries out two-phase laminated flow, obtains organic phase and sour phase, and organic phase returns and aromatic series carboxylic Acid mashing, the nitric acid and sulfuric acid of sour Xiang Yuxin are configured to nitration mixture reuse;
Centrate is isolated 6755g organic phase (dichloroethanes) in phase-splitter, 1411g acid phase.
Embodiment 2
It is with 1 difference of embodiment, the structure of mixed cell are as follows:
First mixed cell of left end is located at 101 lower section of the first import, and the lower bottom part in the first mixed cell has magnetic force Rotor 4,1 lower bottom part of mixing tube outside the first mixed cell have magnetic stirring apparatus 3, are the second mixing lists on the right of the first mixed cell Member, the second mixed cell is by being located at the first overhead gage 201 of its left end and being surrounded positioned at the first lower baffle plate 202 of its right end; Gear 201 is identical with the shapes and sizes of the first lower baffle plate 202 on first;The upper top and mixing tube 1 of first overhead gage 201 The upper top of inner wall is connected, and the lower bottom part 202 of the first lower baffle plate is connected with the lower bottom part of 1 inner wall of mixing tube, keeps off on first The lower bottom part of plate 201 is located at the lower section of 1 cross central line of mixing tube, and the upper top of the first lower baffle plate 202 is located at mixing tube 1 laterally The top of center line;
Third mixed cell, the 4th mixed cell ... .. N mixed cell repeat the structure of the second mixed cell, and N is big In 4 positive integer.
The distance between first overhead gage 201 and the first lower baffle plate 202 are equal in the 2/3 of 201 height of the first overhead gage.
Embodiment 3
It is with the difference of embodiment 1, mixing tube 1 is double layer jacket structure.
The lower-left end of mixing tube 1 has import to be connected with the first collet 208, and the upper right side of mixing tube 1 has outlet and first Collet 208 is connected.Remaining structure is same as Example 1.Mixing tube is arranged to double layer jacket structure, effect is to mixing Material heat preservation in pipe.
Embodiment 4
It is with the difference of embodiment 2, mixing tube 1 is double layer jacket structure.
The lower-left end of mixing tube 1 has import to be connected with the first collet 208, and the upper right side of mixing tube 1 has outlet and first Collet 208 is connected.Remaining structure is same as Example 1.
Mixing tube is arranged to double layer jacket structure, effect is to the material heat preservation in mixing tube.

Claims (10)

1. aromatic carboxy acid compound's nitration reaction equipment therefor, which is characterized in that the device includes mixer and and mixer The tubular reactor being connected further includes glass reaction kettle;
Mixer includes mixing tube, has the first import in the left end of mixing tube, the upper top of left end has the second import, mixing tube There is nitration mixture outlet in rear end, there is multiple mixed cells in mixing tube, and nitration mixture outlet is connected with the import of the left upper end of tubular reactor It connects;
There is agitating device in the left end of tubular reactor, and agitating device includes agitating shaft and blade, and agitating shaft and motor pass through shaft coupling Device is connected and its rotation is driven by motor;
There are multiple temperature sensors, multiple pressure sensors in tubular reactor;
Temperature sensor, pressure sensor are connected with display screen respectively, and display location is on the lateral wall of tubular reactor;
The lower-left end of tubular reactor is provided with drain, is corresponding with valve at drain;
The discharge port of tubular reactor right end is connected with the import of glass reaction kettle, and the right end discharge outlet of tubular reactor has Valve.
2. aromatic carboxy acid compound's nitration reaction equipment therefor as described in claim 1, which is characterized in that mixing tube is double Layer is jacket structured.
3. aromatic carboxy acid compound's nitration reaction equipment therefor as described in claim 1, which is characterized in that a left side for mixing tube Lower end has import to be connected with collet, and the upper right side of mixing tube has outlet to be connected with collet.
4. aromatic carboxy acid compound's nitration reaction equipment therefor as described in claim 1, which is characterized in that the first import with First feed pipe is connected, and the second import is connected with the second feed pipe;There are first flowmeter, the second charging on first feed pipe Guan Shangyou second flowmeter.
5. aromatic carboxy acid compound's nitration reaction equipment therefor as described in claim 1, which is characterized in that tubular reactor It is interior that there are three temperature sensors, three pressure sensors;Temperature sensor and pressure sensor alternate intervals are arranged, adjacent temperature The spacing spent between sensor and pressure sensor is equal.
6. aromatic carboxy acid compound's nitration reaction equipment therefor as described in claim 1, which is characterized in that tubular reactor For double layer jacket structure, there is water inlet at the lower-left end of tubular reactor, and the upper right side of tubular reactor has water outlet.
7. aromatic carboxy acid compound's nitration reaction equipment therefor as described in claim 1, which is characterized in that tubular reactor Internal blade is screw type blade, centered on agitating shaft set by the agitating shaft.
8. aromatic carboxy acid compound's nitration reaction equipment therefor as described in claim 1, which is characterized in that mixed cell Structure is as follows:
First mixed cell of left end is located at below the first import, and the lower bottom part in the first mixed cell has magnetic rotor, the Mixing tube lower bottom part outside one mixed cell has magnetic stirring apparatus, is the second mixed cell on the right of the first mixed cell, and second is mixed It closes unit and is surrounded by being located at the first overhead gage of its left end, the first lower baffle plate and second baffle positioned at its right end;
First overhead gage and the first lower baffle plate shapes and sizes are identical, the first overhead gage and the upper top phase for mixing inside pipe wall Connection, the first lower baffle plate are connected with the lower bottom part of mixing inside pipe wall, and the first overhead gage lower end and the second overhead gage upper end it Between distance it is equal with the first overhead gage/height of the first lower baffle plate;
There are upper mesh areas and lower mesh areas in the upper and lower part of second baffle respectively, and upper mesh areas accounts for the 1/6 of second baffle area, Lower mesh areas accounts for the 1/6 of second baffle area;
Third overhead gage and third lower baffle plate institute of the third mixed cell by being located at the second baffle of its left end and positioned at its right end It surrounds;
Remaining mixed cell repeats the second mixed cell and the structure of third mixed cell is alternately present.
9. aromatic carboxy acid compound's nitration reaction equipment therefor as described in claim 1, which is characterized in that
The structure of mixed cell is as follows: the first mixed cell of left end is located at below the first import, in the first mixed cell Lower bottom part has magnetic rotor, and the mixing tube lower bottom part outside the first mixed cell has magnetic stirring apparatus, is on the right of the first mixed cell Second mixed cell, the second mixed cell is by being located at the first overhead gage of its left end and being enclosed positioned at the first lower baffle plate of its right end At;The shapes and sizes of first overhead gage and the first lower baffle plate are identical;First overhead gage and the upper top for mixing inside pipe wall It is connected, the first lower baffle plate is connected with the lower bottom part of mixing inside pipe wall, and the lower bottom part of the first overhead gage is located at mixing tube transverse direction The lower section of center line, the upper top of the first lower baffle plate are located at the top of mixing tube cross central line;
Third mixed cell, the 4th mixed cell ... .. N mixed cell repeat the structure of the second mixed cell, and N is greater than 4 Positive integer.
10. aromatic carboxy acid compound's nitration reaction equipment therefor as claimed in claim 9, which is characterized in that kept off on first The distance between plate and the first lower baffle plate are at least greater than or equal to the 2/3 of the first overhead gage height.
CN201821963786.7U 2018-11-27 2018-11-27 Aromatic carboxy acid compound's nitration reaction equipment therefor Expired - Fee Related CN209362482U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110860222A (en) * 2019-12-19 2020-03-06 上海弗鲁克科技发展有限公司 Intensified high-viscosity fluid mixing device

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110860222A (en) * 2019-12-19 2020-03-06 上海弗鲁克科技发展有限公司 Intensified high-viscosity fluid mixing device

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