Continuous production technology and device for m-aminoacetanilide

A m-aminoacetanilide, aminoacetanilide technology, applied in the continuous production process and device field of m-aminoacetanilide, can solve the problems of not being able to meet market demand, not being suitable for large-scale production, material and energy loss, etc., and achieve reduction The effect of loss, reduction of labor, reduction of enrichment equipment

Active Publication Date: 2019-04-12
ZHEJIANG DIBANG CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Both of the above two preparation methods use acetic anhydride as an acylating agent, and the price is relatively high. Although the cooling and crystallization process of subsequent products is reduced, the cooling process is still required after the mother liquor is hydrolyzed with acid.
[0006] In addition, the above-mentioned methods are all batch-type kettle-type reactions, and auxiliary operations such as loading and unloading are required in the production process, which is labor-intensive, and at the same time, it is easy to cause loss of materials and energy, and the production cost increases
Batch kettle production is not suitable for large-scale production and cannot meet market demand

Method used

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  • Continuous production technology and device for m-aminoacetanilide

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Experimental program
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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 technology for m-aminoacetanilide. After mother liquor absorbs hydrogen chloride gas, the obtained product, acetic acid and m-phenylenediamine are fed into a primary reaction kettle and subjected to an acylation reaction, and the feeding mas ratio of the fed m-phenylenediamine to the fed hydrogen chloride to the fed acetic acid to the fed mother liquor controlled to be 1:(0.3-0.4):(0.6-0.8):(7-8), one part of materials in the primary reaction kettle is fed into a reaction kettle and cycled, the other part of the materials is fed into a secondaryreaction kettle and reacts, then crystallization and centrifugation are carried out, and a finished product is obtained after treatment. According to the continuous production technology for m-aminoacetanilide, the whole m-aminoacetanilide is produced in a closed system, particularly, non-absorbed hydrogen chloride during the reaction and much acetic-acid waste gas generated when crystallization and centrifugal separation are carried out are absorbed to a final reaction kettle and continue to react, and inorganized gas discharging is reduced; meanwhile comprehensive utilization of resources isachieved, and the yield of the finished product is thus increased.

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

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/43
CPCC07C231/02C07C233/43
Inventor 徐万福周海斌唐智勇冯彦博李勇
Owner ZHEJIANG DIBANG CHEM
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