System and process for continuously producing diazonium salt solution

A diazonium salt and solution technology, applied in chemical instruments and methods, dissolution, organic chemistry, etc., can solve the problems of adaptability improvement of hypergravity reactors, large area of ​​reactors, and few diazonium components, etc. Achieve the effect of enhancing mass transfer effect and residence time, reducing dead angle deposition, mixing and fully reacting

Active Publication Date: 2021-02-19
ZHEJIANG DIBANG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The above-mentioned continuous process adopts the diazotization production process with multiple reactors in series. In order to ensure the complete diazo reaction, more reactors in series are often required, and the reactors occupy a large area.
At the same time, multiple reactors are connected in series, and the overflow method is adopted. There are cases where the diazotization reagent overflows to the next stage while the aromatic amine is still trapped in the upper reactor. Over time, the actual diazo component in the diazo transfer tank is relatively small. , thus affecting the subsequent coupling reaction
[0005] The patent specification with the publication number CN101870824A discloses a technical solution for diazotization reaction using a high-gravity reactor, but it does not improve the adaptability of the high-gravity reactor, and the overall system and process need to be further optimized and improved

Method used

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  • System and process for continuously producing diazonium salt solution
  • System and process for continuously producing diazonium salt solution
  • System and process for continuously producing diazonium salt solution

Examples

Experimental program
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Embodiment 1

[0052] A 1-square pre-mixing tank is used to connect the diazotization reactors in series, the finished product is a 1-square tank, and the stirring speed of the pre-mixing tank is controlled at 300r / min. First, add 300L 28wt% nitrosylsulfuric acid solution (referred to as liquid sub) into the pre-mixing tank, then transport p-nitroaniline to the weighing screw feeder through the pipe chain conveying equipment, and put in p-nitrosylsulfuric acid through the feeder 158kg of aniline, mixed reaction for 30-40 minutes, the temperature of the pre-mixing kettle is controlled at 15-20°C through the jacket and the coil. Subsequently, 150kg / h and 510kg / h of p-nitroaniline and liquid nitrate were respectively fed into the premix tank at the same time, and the temperature of the premix tank was controlled at 15-20°C through a jacket and a coil. The pre-mixed tank is discharged, and fed to the diazotization reactor at a flow rate of 660kg / h through the pump for further diazotization react...

Embodiment 2

[0054] A 1-square pre-mixing tank is used to connect the diazotization reactors in series, the finished product is a 1-square tank, and the stirring speed of the pre-mixing tank is controlled at 400r / min. First, add 300L 28wt% nitrosyl sulfuric acid solution (abbreviated as liquid sub) in the premix tank, then transport 2,4-dinitro-6-chloroaniline to the weighing screw feeder through the screw conveyor, Put 250kg of 2,4-dinitro-6-chloroaniline into the feeder, react for 30 minutes, and control the temperature of the premixing tank at 18-23°C. Subsequently, 2,4-dinitro-6-chloroaniline and liquid sub-alternatives were simultaneously fed into the premix tank at 200kg / h and 420kg / h respectively. The pre-mixed tank is discharged, and fed to the diazotization reactor at a flow rate of 620kg / h through the pump for further diazotization reaction. The speed of the diazotization reactor is 1500rpm, and the diameter of the channel is 0.5mm, spherical The diameter of the cavity is 4mm, t...

Embodiment 3

[0056] A 1-square pre-mixing tank is used to connect the diazotization reactors in series, the finished product is a 1-square tank, and the stirring speed of the pre-mixing tank is controlled at 400r / min. First, add 300L 28wt% nitrosyl sulfuric acid solution (abbreviated as liquid sub) in the premix tank, then transport 2,6-dichloro-4-nitroaniline to the weighing screw feeder through the screw conveyor, Put 250kg of 2,6-dichloro-4-nitroaniline into the feeder, react for 40-50 minutes, and control the temperature of the pre-mixing tank at 20-23°C. Subsequently, 2,6-dichloro-4-nitroaniline and liquid sub-alcohol were simultaneously fed into the premix tank at 200kg / h and 420kg / h respectively. The pre-mixed tank is discharged, and fed to the diazotization reactor at a flow rate of 620kg / h through the pump for further diazotization reaction. The speed of the diazotization reactor is 1800rpm, and the diameter of the channel is 0.5mm, spherical The diameter of the chamber is 4mm, t...

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Abstract

The invention discloses a system and a process for continuously producing a diazonium salt solution. The system comprises conveying equipment, feeding equipment, 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, channels are arranged in astaggered mode, and connecting nodes between the channels are expanded to form a spherical cavity. The process adopts the system and comprises the following steps: (1) uniformly mixing aromatic amineand a diazotization reagent in the premixing kettle, continuously feeding the aromatic amine into the premixing kettle through conveying equipment and feeding equipment under continuous stirring, anddirectly and continuously conveying the diazotization reagent into the premixing kettle at the same time; and (2) continuously feeding and simultaneously continuously discharging the materials from the premixing kettle, enabling the discharged materials to partially flow back to the premixing kettle and partially enter the diazotization reactor, enabling the aromatic amine and the diazotization reagent to fully react, and continuously discharging the diazonium salt solution generated by the reaction to the finished product kettle.

Description

technical field [0001] The invention relates to the technical field of preparation of diazonium components of dyes, in particular to a system and process for continuous production of diazonium salt solution. Background technique [0002] The reaction of aromatic primary amines and nitrous acid (in a strong acid medium) to generate diazonium salts is called diazotization, and the product diazonium salts are widely used in organic synthesis processes such as dyes and medicines, especially in the dye industry, with more than 60% The product is realized by diazotization reaction. [0003] At present, in industrial production, the diazotization reaction mainly adopts the nitrosyl sulfuric acid batch process, that is, in the batch reactor, add nitrosyl sulfuric acid (sometimes need to add more than 80% sulfuric acid solution), and then slowly add aromatic amine . In this process, manual feeding is used, the control is not precise enough, and there are problems such as inconsiste...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/18B01F13/10C07C245/20
CPCB01J19/0066B01J19/18C07C245/20B01F33/80B01F33/8362
Inventor 陈晓栋邹海魁周海斌初广文唐智勇陈建峰徐万福罗勇徐斌孙宝昌张亮亮
Owner ZHEJIANG DIBANG CHEM
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