CN112371072A - System and process for continuously producing diazonium salt solution - Google Patents
System and process for continuously producing diazonium salt solution Download PDFInfo
- Publication number
- CN112371072A CN112371072A CN202011222979.9A CN202011222979A CN112371072A CN 112371072 A CN112371072 A CN 112371072A CN 202011222979 A CN202011222979 A CN 202011222979A CN 112371072 A CN112371072 A CN 112371072A
- Authority
- CN
- China
- Prior art keywords
- kettle
- diazotization
- reactor
- premixing
- continuously
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8362—Mixing plants; Combinations of mixers combining mixing with other treatments with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C245/00—Compounds containing chains of at least two nitrogen atoms with at least one nitrogen-to-nitrogen multiple bond
- C07C245/20—Diazonium compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a system and a process for continuously producing diazonium salt solution, wherein the system comprises a conveying device, a feeding device, a premixing kettle, a diazotization reactor and a finished product kettle which are sequentially connected; the diazotization reactor is a supergravity reactor, a rotating bed with a multi-channel structure is adopted, channels are arranged in a staggered mode, and connecting nodes among the channels are expanded to form spherical cavities. The process adopts the system and comprises the following steps: (1) mixing aromatic amine and diazotization reagent uniformly in a premixing kettle, continuously feeding the aromatic amine into the premixing kettle through a conveying device and a feeding device under the condition of continuous stirring, and simultaneously, directly and continuously conveying the diazotization reagent into the premixing kettle; (2) and continuously discharging while continuously feeding the material in the premixing kettle, wherein part of the discharged material flows back to the premixing kettle, part of the discharged material enters the diazotization reactor, the aromatic amine and the diazotization reagent fully react, and the diazonium salt solution generated by the reaction is continuously discharged to the finished product kettle.
Description
Technical Field
The invention relates to the technical field of preparation of dye diazo components, in particular to a system and a process for continuously producing a diazonium salt solution.
Background
The reaction of aromatic primary amine with nitrous acid (in a strong acid medium) to generate diazonium salt is called diazotization, and the product diazonium salt is widely used in organic synthesis processes of dyes, medicines and the like, particularly in the dye industry, and more than 60 percent of products are realized through diazotization.
At present, in industrial production, a nitrosyl sulfuric acid method batch process is mainly adopted for diazotization, namely nitrosyl sulfuric acid (sometimes more than 80% sulfuric acid solution is required to be added) is added into a batch reactor, and then aromatic amine is slowly added. In the process, the materials are manually fed, the control is not accurate enough, and the problems of inconsistent reaction temperature, unstable reaction working conditions and the like exist. For this purpose, patent CN103664683A discloses a continuous diazotization production process of aromatic amine, namely: adopting a diazo reaction kettle with a plurality of kettles connected in series, putting powdery aromatic amine raw materials into a feed bin of a feeding system, integrally weighing the feeding system and solid raw materials by using a weighing device, continuously and stably feeding the aromatic amine into the diazo reaction kettle by using an automatic feeder, calculating the feeding amount of the aromatic amine in unit time by using a differential method, and according to the feeding molar ratio of the aromatic amine, sulfuric acid and nitrosyl sulfuric acid being 1: (1-5): (1.01-1.1), continuously and stably adding nitrosyl sulfuric acid and sulfuric acid into a diazo kettle through a liquid metering and adjusting device, and carrying out diazotization reaction under stirring at a controlled temperature of 0-40 ℃.
The continuous process adopts a diazotization production process with a plurality of serially connected kettles, and in order to ensure the complete diazotization reaction, a plurality of serially connected reaction kettles are often required, and the occupied area of the reaction kettles is larger. Meanwhile, the multiple kettles are connected in series, and an overflow mode is adopted, so that the diazotization reagent overflows to the next stage, the aromatic amine is still trapped in the upper-stage reaction kettle, and the condition that the actual diazo component of the diazotization transfer tank is less occurs in the long term, thereby influencing the subsequent coupling reaction.
The patent specification with publication number CN101870824A discloses a technical solution for diazotization using a hypergravity reactor, but it does not make any adaptive improvement on the hypergravity reactor, and the overall system and process need further optimization and improvement.
Disclosure of Invention
Aiming at the technical problems and the defects of the existing diazo continuous production system and process in the field, the invention provides a system and process for continuously producing a diazo solution, which can improve the efficiency of diazo continuous production and realize the stability of product quality.
A system for continuously producing diazonium salt solution comprises a conveying device, a feeding device, a premixing kettle, a diazotization reactor and a finished product kettle which are connected in sequence;
the diazotization reactor is a supergravity reactor, a multi-channel structure rotating bed is adopted, the channels are arranged in a staggered mode, and connecting nodes among the channels are expanded to form spherical cavities.
The diazotization reactor can be one of a vertical type and a horizontal type.
Before the materials enter the diazotization reactor, a premixing kettle device is installed, so that the problem that the diazotization reactor (a supergravity reactor) cannot feed particles or powder is solved.
The existing hypergravity reactor can not simultaneously consider mass transfer effect and retention time, and if strong mass transfer effect is needed, the rotating speed is increased, but the corresponding retention time is shortened, and if the retention time is increased, the rotating speed is reduced, but the mass transfer effect is weakened. Thus, existing hypergravity reactors typically require a recycle operation to achieve both mass transfer/mixing and increased material residence time.
The invention adopts the special multi-channel structure rotating bed, does not need circulating materials, reduces the mixing dead zone, can ensure that reaction materials have more chances to contact with each other in the reaction channel, strengthens the mixing of two materials, enhances the impact action, forms larger turbulent kinetic energy, and further improves the reaction rate. The spherical cavity formed by expanding the channel port has the functions of temporarily converging materials and redistributing the materials, reduces the deposition of the materials in dead angles of the reaction channel, avoids the condition of pipeline blockage, prolongs the retention time of the materials to a certain extent, and ensures more sufficient mixing and reaction.
The invention adopts a special multi-channel structure rotating bed, overcomes the technical problem that the existing hypergravity reactor can not simultaneously consider both mass transfer effect and retention time, and increases the retention time of reaction materials while ensuring strong mass transfer effect.
The pipe diameter of the channel is preferably 0.5-2 mm, and the diameter of the spherical cavity is preferably 4-8 mm.
Preferably, the conveying device is a closed device, and can be a pneumatic conveying device, a conveyor belt, a screw feeder, a vacuum conveying device and the like. The conveying equipment conveys the aromatic amine to the feeding equipment, so that manual operation is reduced, and the production efficiency is improved. The conveying equipment is closed, so that the problem that aromatic amine powder solid materials such as 2, 4-dinitro-6-chloro (bromo) aniline, 2, 6-dichloro-p-nitroaniline and the like are easy to scatter everywhere can be avoided, the loss of raw materials is reduced, and the production environment is improved.
Preferably, the feeding equipment is provided with a weighing module and a variable frequency control module, the instantaneous feeding amount is calculated through the change of a weighing value in unit time before and after, and the feeding speed is changed through the setting of variable frequency. The feeding equipment can be a weighing screw feeder, a weighing vibration feeder and the like.
Further preferably, the conveying equipment and a weighing module of the feeding equipment are in interlocking control.
Preferably, the premixing kettle is provided with a jacket, and a coil is arranged in the jacket and used for controlling the temperature.
Preferably, a stirring paddle and a demister are arranged in the premixing kettle. More preferably, the demister is arranged at 1/3-2/3 positions of the stirring paddle from bottom to top. The invention is provided with the foam remover, thereby greatly reducing the foam generated by stirring, particularly the excessive foam of the diazotization reaction, which can influence the quality of the product diazonium salt solution and the accurate measurement of the feeding.
Preferably, the channels are arranged in a criss-cross three-dimensional staggered manner.
Preferably, the diazotization reactor is provided with a jacket, and a coil is arranged in the jacket and used for controlling the temperature.
The invention also provides a process for continuously producing the diazonium salt solution, and the system for continuously producing the diazonium salt solution comprises the following steps:
(1) mixing aromatic amine and diazotization reagent uniformly in a premixing kettle, continuously feeding the aromatic amine into the premixing kettle through a conveying device and a feeding device under the condition of continuous stirring, and simultaneously, directly and continuously conveying the diazotization reagent into the premixing kettle;
(2) and continuously discharging while continuously feeding the material in the premixing kettle, wherein part of the discharged material flows back to the premixing kettle, part of the discharged material enters the diazotization reactor, the aromatic amine and the diazotization reagent fully react under the effect of supergravity, and the diazonium salt solution generated by the reaction is continuously discharged to the finished product kettle.
Preferably, in the step (1), the diazotizing agent is 28-40 wt% of nitrosyl sulfuric acid solution or contains 28-40 wt% of nitrosyl sulfuric acid and more than 80 wt% of H2SO4The mixed solution of (1).
Further excellenceOptionally, the aromatic amine, nitrosylsulfuric acid and H2SO4The molar ratio of (A) to (B) is 1:1 to 1.3:0 to 10.
The aromatic amine can be one or two of aromatic primary amines or heterocyclic amines substituted by aniline, halogen, nitro and cyano, in particular p-nitroaniline, o-chloro-p-nitroaniline, o-bromo-p-nitroaniline, o-cyano-p-nitroaniline, 2, 6-dichloro-4-nitroaniline, 2, 6-dibromo-4-nitroaniline, 2, 6-dicyano-4-nitroaniline, 2, 4-dinitro-6-chloroaniline, 2, 4-dinitro-6-bromoaniline, 6-nitro-2-aminobenzothiazole, 5-nitro-3-aminobenzothiazole, 2-amino-5, 6-dichlorobenzothiazole and the like.
In the step (1), the mixing of the reaction medium and the mass and heat transfer can be accelerated by rapidly stirring in the premixing kettle. In the step (1), the rotation speed of the stirring is preferably 100 to 800rpm, and more preferably 200 to 400 rpm.
Preferably, in the step (1), the temperature in the premixing kettle is controlled to be-10 to 30 ℃. Further preferably, the temperature in the premixing kettle is controlled to be-10-25 ℃.
Preferably, in the step (2), the ratio of the discharge material refluxed to the premixing kettle to the discharge material entering the diazotization reactor is 2-5: 10.
The method is matched with a special multi-channel structure rotating bed, and in the step (2), the rotating speed of the diazotization reactor is preferably 100-10000 rpm, more preferably 800-3000 rpm, and even more preferably 1000-2500 rpm. The rotating speed is too high, the centrifugal force borne by the reaction materials is too large, the residence time in the rotating bed is shortened, and the energy consumption of equipment is increased; the rotating speed is too slow, and the reaction strengthening effect cannot be achieved.
Preferably, the reaction temperature in the diazotization reactor is controlled to be-10-30 ℃.
As a general inventive concept, the invention also provides a hypergravity reactor, which adopts a multi-channel structure rotating bed, the channels are arranged in a staggered way, and the connecting nodes between the channels are expanded to form spherical cavities.
Compared with the prior art, the invention has the main advantages that:
1. the reaction materials are premixed and then fed into a diazotization reactor (a hypergravity reactor), and the reaction materials are combined with a channel with a special structure through hypergravity, and meanwhile, the mass transfer effect and the retention time of the reaction materials are enhanced, so that the diazotization reaction is accelerated, and the occupied area of a common kettle type reactor is reduced;
2. by the continuous operation of feeding and the like, the problems of unstable reaction working condition, high operation intensity of workers and the like in intermittent production can be greatly improved;
3. by using a closed conveying device and the like, the problem that powder solid materials such as 2, 4-dinitro-6-chloro (bromo) aniline, 2, 6-dichloro-p-nitroaniline and the like are easy to scatter everywhere can be avoided, the loss of raw materials is reduced, and the production environment is improved.
Drawings
FIG. 1 is a schematic view of a system for continuously producing a diazonium salt solution according to the present invention;
FIG. 2 is a schematic front view of a diazotization reactor according to the present invention;
FIG. 3 is a schematic structural view of a multi-channel structure rotating bed of the present invention;
in the figure: 1-conveying equipment, 2-feeding equipment, 3-premixing kettle, 4-diazotization reactor, 5-finished product kettle, 6-multichannel structure rotating bed, 7-spherical cavity, 8-channel and 9-rotating shaft.
Detailed Description
The invention is further described with reference to the following drawings and specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are conducted under conditions not specified, usually according to conventional conditions, or according to conditions recommended by the manufacturer.
The system for continuously producing the diazonium salt solution is shown in figure 1 and comprises a conveying device 1, a feeding device 2, a premixing kettle 3, a diazotization reactor 4 and a finished product kettle 5 which are connected in sequence.
The conveying device 1 is a closed device and is used for continuously conveying aromatic amine solids.
The feeding equipment 2 is provided with a weighing module and a variable frequency control module, the instantaneous feeding amount is calculated through the change of a weighing numerical value in unit time, and the feeding speed is changed through the setting of variable frequency.
The conveying equipment 1 and the weighing module of the feeding equipment 2 are controlled in an interlocking way.
The premixing kettle 3 is provided with a jacket, and a coil pipe is arranged in the jacket and used for controlling the temperature. The inside of the premixing kettle 3 is provided with a stirring paddle and a demister. The discharge pipe at the bottom of the premixing kettle 3 is respectively connected with the reflux port at the top of the premixing kettle 3 and the feed inlet at the top of the diazotization reactor 4 through a pump.
The structure of the diazotization reactor 4 is shown in figure 2, the top is used for feeding, a circular multi-channel structure rotating bed 6 is arranged in an upper cavity, and a driving motor is arranged at the bottom. The rotating shaft 9 is connected to the bottom of the multi-channel structure rotating bed 6, and the rotating shaft 9 is driven to rotate by the driving motor, so that the rotating bed 6 is driven to rotate by taking the rotating shaft 9 as an axis. Due to the centrifugal action, the material is discharged from the side surface of the rotating bed 6 and finally enters the finished product kettle through the material outlet of the diazotization reactor 4.
The structure of the multi-channel structure rotating bed 6 is shown in figure 3, feeding is carried out at the top of the middle, internal channels 8 are criss-cross in three dimensions, and connecting nodes among the channels 8 are expanded to form a spherical cavity 7. After entering the channel 8, the material simultaneously performs circular motion and radial motion under the action of rotary centrifugation, and the reinforced mixing reaction and redistribution process are repeatedly performed in the channel 8 and the spherical cavity 7, and finally the material is discharged from the side surface of the multi-channel structure rotating bed 6.
The above-described system for continuously producing a diazonium salt solution was used in each of examples 1 to 3.
Example 1
A1-square premixing kettle is adopted to be connected with a diazotization reactor in series, a finished product kettle is a 1-square kettle, and the stirring speed of the premixing kettle is controlled at 300 r/min. Firstly, adding 300L of 28 wt% nitrosyl sulfuric acid solution (liquid nitrite for short) into a premixing kettle, then conveying p-nitroaniline to a weighing screw feeder through pipe chain conveying equipment, adding 158kg of p-nitroaniline through the feeder, mixing and reacting for 30-40 minutes, and controlling the temperature of the premixing kettle at 15-20 ℃ through a jacket and a coil pipe. And then, simultaneously feeding the paranitroaniline and the liquid ammonia into a premixing kettle according to 150kg/h and 510kg/h respectively, and controlling the temperature of the premixing kettle to be 15-20 ℃ through a jacket and a coil pipe. Discharging the material from the premixing kettle, feeding the material into a diazotization reactor for further diazotization reaction through a pump according to the flow rate of 660kg/h, controlling the temperature of the reactor to be 25-28 ℃ and the flow rate of 140kg/h to be pumped back to the premixing kettle, wherein the rotating speed of the diazotization reactor is 1800rpm, the diameter of a channel pipe is 1mm, the diameter of a spherical cavity is 6mm, and the reactor is discharged to a 1-square reaction kettle for subsequent coupling reaction. No p-nitroaniline particles are found in the detection of the freezing point of the product.
Example 2
A1-square premixing kettle is adopted to be connected with a diazotization reactor in series, a finished product kettle is a 1-square kettle, and the stirring speed of the premixing kettle is controlled at 400 r/min. Firstly, adding 300L of 28 wt% nitrosyl sulfuric acid solution (called Liya for short) into a premixing kettle, then conveying the 2, 4-dinitro-6-chloroaniline to a weighing screw feeder through a screw conveyor, adding 250kg of the 2, 4-dinitro-6-chloroaniline through the feeder, reacting for 30 minutes, and controlling the temperature of the premixing kettle at 18-23 ℃. Then, the 2, 4-dinitro-6-chloroaniline and the liquid ammonia are simultaneously fed into a premixing kettle according to 200kg/h and 420kg/h respectively. Discharging the material from the premixing kettle, feeding the material into a diazotization reactor for further diazotization reaction through a pump according to the flow rate of 620kg/h, controlling the temperature to be 25-28 ℃ and the rotation speed of the diazotization reactor to be 1500rpm, controlling the pipe diameter of a channel to be 0.5mm, controlling the diameter of a spherical cavity to be 4mm, and pumping the material back to the premixing kettle at the speed of 200kg/h, wherein the material is discharged to a 1-square reaction kettle and is used for subsequent coupling reaction. No 2, 4-dinitro-6-chloroaniline particles are found in the detection of the freezing point of the product.
Example 3
A1-square premixing kettle is adopted to be connected with a diazotization reactor in series, a finished product kettle is a 1-square kettle, and the stirring speed of the premixing kettle is controlled at 400 r/min. Firstly, adding 300L of 28 wt% nitrosyl sulfuric acid solution (liquid nitrite for short) into a premixing kettle, then conveying the 2, 6-dichloro-4-nitroaniline to a weighing type screw feeder through a screw conveyor, adding 250kg of the 2, 6-dichloro-4-nitroaniline through the feeder, reacting for 40-50 minutes, and controlling the temperature of the premixing kettle at 20-23 ℃. Subsequently, the 2, 6-dichloro-4-nitroaniline and the Liya were simultaneously fed into a premixing kettle at 200kg/h and 420kg/h, respectively. Discharging the material from the premixing kettle, feeding the material into a diazotization reactor for further diazotization reaction through a pump according to the flow rate of 620kg/h, wherein the rotating speed of the diazotization reactor is 1800rpm, the pipe diameter of a channel is 0.5mm, the diameter of a spherical cavity is 4mm, the temperature of the reactor is controlled to be 25-28 ℃, in addition, 190kg/h of the material is pumped back to the premixing kettle, and the material is discharged to a 1-square reaction kettle for subsequent coupling reaction. No 2, 6-dichloro-4-nitroaniline particles are found in the detection of the freezing point of the product.
Comparative example 1
Adopting a traditional conventional batch reaction kettle to prepare a diazonium salt solution, adopting a 5-party reaction kettle, adding 4400kg of liquid ammonia under stirring, opening frozen brine, cooling to 10-15 ℃, then slowly adding 1300kg of p-nitroaniline in batches, wherein the whole feeding time is 8 hours, and after the feeding is finished, keeping the temperature at 20-25 ℃ for 5 hours, no p-nitroaniline particulate matter is detected in the detection of the freezing point of the product.
Comparative example 2
Preparing a diazonium salt solution by adopting a conventional intermittent reaction kettle, adding 4200kg of liquid ammonia under stirring by adopting a 5-square reaction kettle, opening frozen brine, cooling to 20-25 ℃, then slowly adding 2100kg of 2, 4-dinitro-6-chloroaniline in batches, wherein the whole feeding time is 8 hours, and after the feeding is finished, keeping the temperature for 6 hours at 28-30 ℃, and detecting the freezing point of a product to find no 2, 4-dinitro-6-chloroaniline particulate matter.
Comparative example 3
A1-square premixing kettle is connected in series with a conventional hypergravity reactor, a rotating bed of the reactor adopts a conventional spiral channel structure, a finished product kettle is a 1-square kettle, and the stirring speed of the premixing kettle is controlled at 400 r/min. Firstly, adding 300L of 28 wt% nitrosyl sulfuric acid solution (called Liya for short) into a premixing kettle, then conveying the 2, 4-dinitro-6-chloroaniline to a weighing screw feeder through a screw conveyor, adding 250kg of the 2, 4-dinitro-6-chloroaniline through the feeder, reacting for 30 minutes, and controlling the temperature of the premixing kettle at 18-23 ℃. Then, the 2, 4-dinitro-6-chloroaniline and the liquid ammonia are simultaneously fed into a premixing kettle according to 200kg/h and 420kg/h respectively. Discharging the material from the premixing kettle, feeding the material into a conventional supergravity reactor for further diazotization reaction through a pump according to the flow rate of 620kg/h, wherein the rotating speed of the conventional supergravity reactor is 1500rpm, the distance between spiral channels is 5mm, the temperature of the reactor is controlled to be 25-28 ℃, in addition, the material is pumped back to the premixing kettle at the speed of 200kg/h, discharging the material from the reactor to a reaction kettle of 1 square for standby, and detecting the freezing point of the product to find that unreacted 2, 4-dinitro-6-chloroaniline particles exist.
From examples 1 and 2, the yields of the diazonium salt solution per unit time of the invention are respectively 660kg/h and 620kg/h, and the yields of the diazonium salt solution per unit time of the comparative examples 1 and 2 are respectively 438kg/h and 450kg/h, so that compared with an intermittent process, the production efficiency of the diazonium salt solution is greatly improved, the process is stable, the loss of raw materials is less, and the problem that the aromatic amine floats everywhere is avoided. By comparing example 2 with comparative example 3, it can be seen that the reaction efficiency is higher and the reaction is more thorough with the multi-channel structure rotating bed of the present invention than the conventional spiral channel rotating structure with the same feeding amount. The multi-channel structure rotating bed structure is suitable for large-scale industrial production.
Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the above description of the present invention, and equivalents also fall within the scope of the invention as defined by the appended claims.
Claims (12)
1. A system for continuously producing diazonium salt solution is characterized by comprising a conveying device, a feeding device, a premixing kettle, a diazotization reactor and a finished product kettle which are sequentially connected;
the diazotization reactor is a supergravity reactor, a multi-channel structure rotating bed is adopted, the channels are arranged in a staggered mode, and connecting nodes among the channels are expanded to form spherical cavities.
2. The system of claim 1, wherein the diameter of the channel is 0.5-2 mm, and the diameter of the spherical cavity is 4-8 mm.
3. The system of claim 1, wherein the delivery apparatus is a containment apparatus.
4. The system as claimed in claim 1 or 3, wherein the feeding device is provided with a weighing module and a variable frequency control module, the instantaneous feeding amount is calculated through the change before and after the weighing value in unit time, and the feeding speed is changed through the setting of variable frequency.
5. The system of claim 4, wherein the conveyor apparatus is interlockingly controlled with a weighing module of the charging apparatus.
6. The system of claim 1, wherein the premix kettle is jacketed with coiled tubing disposed therein;
a stirring paddle and a demister are arranged in the premixing kettle, and the demister is arranged at 1/3-2/3 of the stirring paddle from bottom to top.
7. The system of claim 1, wherein the channels are arranged in a criss-cross three-dimensional staggered arrangement;
the diazotization reactor is provided with a jacket, and a coil pipe is arranged in the jacket.
8. A process for the continuous production of diazonium salt solutions, characterised in that it uses a system according to any one of claims 1 to 7, comprising the steps of:
(1) mixing aromatic amine and diazotization reagent uniformly in a premixing kettle, continuously feeding the aromatic amine into the premixing kettle through a conveying device and a feeding device under the condition of continuous stirring, and simultaneously, directly and continuously conveying the diazotization reagent into the premixing kettle;
(2) and continuously discharging while continuously feeding the material in the premixing kettle, wherein part of the discharged material flows back to the premixing kettle, part of the discharged material enters the diazotization reactor, the aromatic amine and the diazotization reagent fully react under the effect of supergravity, and the diazonium salt solution generated by the reaction is continuously discharged to the finished product kettle.
9. The process according to claim 8, wherein in step (1), the diazotizing agent is 28-40 wt% nitrosyl sulfuric acid solution or contains 28-40 wt% nitrosyl sulfuric acid and more than 80 wt% H2SO4The mixed solution of (1);
said fragranceAmine, nitrosylsulfuric acid and H2SO4The molar ratio of (A) to (B) is 1:1 to 1.3:0 to 10.
10. The process according to claim 8 or 9, wherein in the step (1), the rotating speed of the stirring is 100-800 rpm, and the temperature in the premixing kettle is controlled to be-10-30 ℃;
in the step (2), the ratio of the discharge material refluxed to the premixing kettle to the discharge material entering the diazotization reactor is 2-5: 10.
11. The process according to claim 8, wherein in the step (2), the rotating speed of the diazotization reactor is 100-10000 rpm, and the reaction temperature in the diazotization reactor is controlled to be-10-30 ℃.
12. A hypergravity reactor is characterized in that a multi-channel structure rotating bed is adopted, channels are arranged in a staggered mode, and connecting nodes among the channels are expanded to form spherical cavities.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011222979.9A CN112371072B (en) | 2020-11-05 | 2020-11-05 | System and process for continuously producing diazonium salt solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011222979.9A CN112371072B (en) | 2020-11-05 | 2020-11-05 | System and process for continuously producing diazonium salt solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112371072A true CN112371072A (en) | 2021-02-19 |
| CN112371072B CN112371072B (en) | 2021-08-10 |
Family
ID=74578333
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011222979.9A Active CN112371072B (en) | 2020-11-05 | 2020-11-05 | System and process for continuously producing diazonium salt solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112371072B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527136A (en) * | 2021-08-19 | 2021-10-22 | 浙江迪邦化工有限公司 | System and process for producing paranitroaniline diazonium salt |
| CN113816859A (en) * | 2021-08-23 | 2021-12-21 | 浙江迪邦化工有限公司 | Method for continuously producing 6-chloro-2, 4-dinitroaniline and diazonium salt thereof |
| CN115282913A (en) * | 2022-08-12 | 2022-11-04 | 中国海洋石油集团有限公司 | Reaction system and method for preparing methyl propionate |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594279A (en) * | 2004-06-29 | 2005-03-16 | 浙江大学 | Process and apparatus for producing o-phenylenediamine |
| CN101870824A (en) * | 2010-06-08 | 2010-10-27 | 北京化工大学 | Method for preparing azo colouring agent by utilizing supergravity reactor |
| CN103664683A (en) * | 2012-09-21 | 2014-03-26 | 浙江龙盛集团股份有限公司 | Continuous diazotization production process of aromatic amine |
| CN104529689A (en) * | 2015-01-26 | 2015-04-22 | 深圳市一正科技有限公司 | Preparation method of 9,9,10,10-tetraphenyl-9,10-deoxyanthraquinone |
| CN208161443U (en) * | 2018-03-29 | 2018-11-30 | 响水县玉帛纺织有限公司 | A kind of Textile Dyes pre-mixing apparatus |
| CN109173949A (en) * | 2018-08-07 | 2019-01-11 | 浙江大学 | A kind of closed injection pump promotees to mix micro-fluidic reaction unit and method |
| CN109603702A (en) * | 2018-12-03 | 2019-04-12 | 安徽科技学院 | A kind of hypergravity-divides shape to hit bed reactor |
| CN109651843A (en) * | 2019-01-21 | 2019-04-19 | 北京化工大学 | The continuous production system of the azo active dyestuff of hypergravity |
| CN110449103A (en) * | 2019-07-29 | 2019-11-15 | 浙江迪邦化工有限公司 | A kind of integration system of band premix for diazonium salt method and apparatus |
| EP3590885A1 (en) * | 2018-07-05 | 2020-01-08 | Karlsruher Institut für Technologie | Composite material comprising dna hydrogel and silica nanoparticles |
| CN211358788U (en) * | 2019-09-25 | 2020-08-28 | 浙江华科化工设备有限公司 | Fixed valve concentric ring rotating bed |
-
2020
- 2020-11-05 CN CN202011222979.9A patent/CN112371072B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594279A (en) * | 2004-06-29 | 2005-03-16 | 浙江大学 | Process and apparatus for producing o-phenylenediamine |
| CN101870824A (en) * | 2010-06-08 | 2010-10-27 | 北京化工大学 | Method for preparing azo colouring agent by utilizing supergravity reactor |
| CN103664683A (en) * | 2012-09-21 | 2014-03-26 | 浙江龙盛集团股份有限公司 | Continuous diazotization production process of aromatic amine |
| CN104529689A (en) * | 2015-01-26 | 2015-04-22 | 深圳市一正科技有限公司 | Preparation method of 9,9,10,10-tetraphenyl-9,10-deoxyanthraquinone |
| CN208161443U (en) * | 2018-03-29 | 2018-11-30 | 响水县玉帛纺织有限公司 | A kind of Textile Dyes pre-mixing apparatus |
| EP3590885A1 (en) * | 2018-07-05 | 2020-01-08 | Karlsruher Institut für Technologie | Composite material comprising dna hydrogel and silica nanoparticles |
| CN109173949A (en) * | 2018-08-07 | 2019-01-11 | 浙江大学 | A kind of closed injection pump promotees to mix micro-fluidic reaction unit and method |
| CN109603702A (en) * | 2018-12-03 | 2019-04-12 | 安徽科技学院 | A kind of hypergravity-divides shape to hit bed reactor |
| CN109651843A (en) * | 2019-01-21 | 2019-04-19 | 北京化工大学 | The continuous production system of the azo active dyestuff of hypergravity |
| CN110449103A (en) * | 2019-07-29 | 2019-11-15 | 浙江迪邦化工有限公司 | A kind of integration system of band premix for diazonium salt method and apparatus |
| CN211358788U (en) * | 2019-09-25 | 2020-08-28 | 浙江华科化工设备有限公司 | Fixed valve concentric ring rotating bed |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527136A (en) * | 2021-08-19 | 2021-10-22 | 浙江迪邦化工有限公司 | System and process for producing paranitroaniline diazonium salt |
| CN113527136B (en) * | 2021-08-19 | 2023-08-04 | 浙江迪邦化工有限公司 | System and process for producing diazonium salt of p-nitroaniline |
| CN113816859A (en) * | 2021-08-23 | 2021-12-21 | 浙江迪邦化工有限公司 | Method for continuously producing 6-chloro-2, 4-dinitroaniline and diazonium salt thereof |
| CN115282913A (en) * | 2022-08-12 | 2022-11-04 | 中国海洋石油集团有限公司 | Reaction system and method for preparing methyl propionate |
| CN115282913B (en) * | 2022-08-12 | 2024-01-09 | 中国海洋石油集团有限公司 | Reaction system and method for preparing methyl propionate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112371072B (en) | 2021-08-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112371072B (en) | System and process for continuously producing diazonium salt solution | |
| CN110449103B (en) | Method and device for integrally preparing diazonium salt with premixing function | |
| CN110508231B (en) | Continuous production system of azo reactive dye applying supergravity | |
| CN109893880B (en) | Continuous multi-stage constant temperature difference cooling crystallizer | |
| CN109651843B (en) | Continuous production system of azo reactive dye applying supergravity | |
| CN112592365A (en) | Method for producing acyl thiosilane | |
| CN211435164U (en) | Continuous crystallization process unit of sodium bisulfite menadione | |
| CN218452143U (en) | Continuous circulating grinding system for high-temperature alpha alumina micropowder production | |
| CN218901857U (en) | Device for continuously producing high-solid-content polymer products | |
| CN209997613U (en) | Reaction kettle for preparing precursor of ternary cathode material | |
| CN110433755B (en) | Method and device for continuously preparing diazo compound | |
| CN213674748U (en) | Concrete production system | |
| CN109651842B (en) | Continuous production method of azo reactive dye by using supergravity | |
| CN112592602A (en) | Continuous production system of nano disperse dye | |
| CN210308521U (en) | Plastic particle stirring device | |
| CN101054473B (en) | Coupling producing device and producing technique | |
| CN206188689U (en) | Continuous production unit of diazo -reaction | |
| CN220657139U (en) | Granulating fertilizer raw material mixing stirring equipment | |
| CN220780148U (en) | Multi-stage mixing system for powdery fertilizer raw materials | |
| CN105268392A (en) | Dye synthesis reaction kettle | |
| CN213131998U (en) | Cobalt sulfate crystallization device | |
| CN104830089A (en) | Dye continuous coupling method with reduced energy consumption | |
| CN215277296U (en) | Reation kettle of abundant reaction | |
| CN215138728U (en) | Mixer capable of replacing reaction kettle | |
| CN2936413Y (en) | High efficiency stirrer of high tower prilling smelting slurry mixing bath |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |