A continuous production process and device for m-aminoacetanilide

A technology of aminoacetanilide and production process, which is applied in the field of continuous production process and device of m-aminoacetanilide, can solve the problems such as inability to meet market demands, unsuitable for large-scale production, loss of materials and energy, and reduce steam consumption , The effect of reducing the concentration equipment and improving the efficiency

A technology of aminoacetanilide and production process, which is applied in the field of continuous production process and device of m-aminoacetanilide, can solve the problems such as inability to meet market demands, unsuitable for large-scale production, loss of materials and energy, and reduce steam consumption , The effect of reducing the concentration equipment and improving the efficiency

CN109608353BActive Publication Date: 2021-05-25ZHEJIANG DIBANG CHEM
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  • A continuous production process and device for m-aminoacetanilide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Such as figure 1 As shown, using three-stage series reactors (1, 2, 3), three-stage series crystallization kettles (4, 5, 6), four parallel centrifuges (7, 8, 9) and two mother liquor water collection tanks (10, 11), the volumes of the three reactors are all 10m 3 , the volume of the three crystallization tanks is 12.5m 3 , the volume of the two mother liquid water collection tanks is 100m 3 , the volume of the four centrifuges is 1m 3 .

[0036] The mother liquid water is controlled by a regulating valve and a flow meter, pumped into the absorption tower at 2100kg / h, and hydrogen chloride gas enters the absorption tower at 120kg / h. After the mother liquid is thickened, it is continuously discharged through the discharge pump at the bottom of the absorption tower and mixed with acetic acid It also enters the heat exchanger of the first-stage reactor for preheating, and the flow rate of acetic acid is 240 kg / h.

[0037] After preheating, the mixed solution with a te...

Embodiment 2

[0042] According to the operating method described in Example 1, the difference is the flow rate of raw materials: m-phenylenediamine, hydrogen chloride, acetic acid, mother liquor water feed rate are respectively 370kg / h, 130kg / h, 240kg / h, 2595kg / h; The first-stage reactor enters the next-stage reactor at a flow rate of 3330kg / h, the third-stage reactor enters the first-stage crystallization kettle at a flow rate of 3330kg / h, and the third-stage crystallization kettle cools down to 26°C and enters the centrifuge at a flow rate of 3330kg / h.

[0043] The purity of the m-aminoacetanilide product obtained by centrifugation is 99.21% (HPLC), and the product of m-aminoacetanilide hydrochloride can be obtained in 30 hours of continuous production with a dry weight of 18.2T.

Embodiment 3

[0045] According to the operation method described in Example 2, the difference is that: the reaction kettle adopts 4 stages in series, the purity of the m-aminoacetanilide product obtained by centrifugation is 99.56% (HPLC), and the m-aminoacetanilide hydrochloride product can be obtained in 30 hours of continuous production Fold dry 17.5T.

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Abstract

The invention discloses a continuous production process of m-aminoacetanilide. After absorbing hydrogen chloride gas, the mother liquid water enters the first-stage reaction kettle with acetic acid and m-phenylenediamine for acylation reaction, and the m-phenylenediamine and hydrogen chloride entering are controlled. , The feed mass ratio of acetic acid and mother liquid water is 1: 0.3-0.4: 0.6-0.8: 7-8. Part of the material in the upper-stage reactor is circulated in its own reactor through the pump, and the other part enters the next-stage reaction. The kettle continues to react, and then undergoes crystallization, centrifugation, and processing to obtain the finished product. The whole process of the present invention is produced in a closed system, especially when reacting unabsorbed hydrogen chloride, crystallization, and centrifugation, more acetic acid waste gas is absorbed to the final reactor to continue to participate in the reaction, reducing the discharge of unorganized gas and realizing It improves the comprehensive utilization of resources and further improves the yield of finished products.

Description

technical field [0001] The invention relates to a production process of a dye intermediate, in particular to a continuous production process and device of m-aminoacetanilide. Background technique [0002] M-Aminoacetanilide is a widely used chemical raw material, which is widely used as an intermediate for rapid dyes and medicines, mainly for the preparation of reactive yellow K-RN and disperse dyes, and is in great demand. The synthesis method usually uses acetic acid (or acetic anhydride), hydrochloric acid, and m-phenylenediamine as raw materials, and heats the reaction at about 90 ° C. After the reaction is completed, the temperature is lowered to crystallize, filtered, and the separated mother liquor water is subjected to vacuum distillation and concentration. next batch. [0003] Due to the problems of cumbersome steps and high energy consumption in the above-mentioned traditional method, Chinese patent application document CN101328133A discloses a synthesis method of...

Claims

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Application Information

Patent Timeline
25 May 2021
Publication
CN109608353B
IPC
C07C231/02; C07C233/43
CPC
C07C231/02; C07C233/43
Inventors
徐万福; 周海斌