Technology for separating and purifying 2,4-diaminotoluene and 2,6-diaminotoluene by derivatization crystallization process

A technology of diaminotoluene and crystallization, which is applied in the purification/separation of amino compounds, organic chemistry and other directions, can solve the problems of low recovery rate, large waste of raw materials, serious environmental pollution, etc., and achieves low production cost, convenient operation and simple process. Effect

Inactive Publication Date: 2013-09-25
GANSU SHANDAN HONGDINGYUAN CHEM
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  • Application Information

AI Technical Summary

Problems solved by technology

Domestic manufacturers of 2,4-diaminotoluene mostly use 2,4-dinitrotoluene to reduce 2,4-diaminotoluene with iron powder under acidic conditions to produce 2,4-diaminotoluene. During the production process, a large amount of acidic wastewater, waste residue, causing serious environmental pollution, therefore, the process of producing 2,4-diaminotoluene with this method is gradually being eliminated
In addition, very few domestic manufacturers use double-effect process distillation to produce 2,4-diaminotoluene by high-vacuum distillation of TDA at high temperature, but this process has disadvantages such as low recovery rate and large waste of raw materials.
At the same time, after extracting 2,4-diaminotoluene, a large amount of mixture of 2,4-diaminotoluene and 2,6-diaminotoluene will remain. The content of the two components in the mixture is about 50% each. Purification produces a large amount of waste residue, and the environmental pollution is also very serious

Method used

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  • Technology for separating and purifying 2,4-diaminotoluene and 2,6-diaminotoluene by derivatization crystallization process
  • Technology for separating and purifying 2,4-diaminotoluene and 2,6-diaminotoluene by derivatization crystallization process

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Embodiment Construction

[0015] (1) Rectification of TDA raw materials to remove tar, water, solvent and other impurities

[0016] Using diaminotoluene TDA (a mixture of 80% 2,4-diaminotoluene and 20% 2,6-diaminotoluene) purchased on the market as raw material, the TDA raw material is first crushed, put into a rectifying tower and separated Segment rectification treatment to separate impurities such as moisture, tar and solvents in different amounts contained in the raw material to obtain TDA raw material with a certain purity.

[0017] (2) Crystallization separation and secondary purification of 2,6-diaminotoluene

[0018] Put the raw material TDA after rectification and degumming treatment into distilled water (the mass ratio of solid to liquid is 1:15~1:20), add hydrochloric acid to adjust the pH=6~6.5, and then add sodium chloride with a dosage of 3~5% of raw material TDA , heated to 95~97°C, stirring the catalytic reaction for 0.5~1 hour under the condition of keeping the temperature consta...

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Abstract

The invention provides a technology for separating and purifying 2,4-diaminotoluene and 2,6-diaminotoluene by a derivatization crystallization process. The technology adopts TDA as a raw material and comprises the following steps of: performing rectification degumming treatment and dissolving in distilled water; adjusting the pH to 6-6.5, adding sodium chloride and performing a catalysis reaction; crystallizing and separating to obtain a crude product of 2,6-diaminotoluene; performing sectional rectification to obtain a pure product of 2,6-diaminotoluene; adjusting the pH of the mother liquid obtained after separating the 2,6-diaminotoluene to 10-12; adding sodium hydrosulfite and performing a catalysis reaction; crystallizing and separating to obtain a crude product of 2,4-diaminotoluene; performing sectional rectification to obtain a pure product of 2,4-diaminotoluene. According to the technology provided by the invention, a derivatization crystallization process is adopted for separation and purification so that the 2,4-diaminotoluene and 2,6-diaminotoluene in TDA (Toluene Diammonium) are completely separated, the utilization rate of the raw materials is over 99%, and the main content of the product is over 99%.

Description

technical field [0001] The invention belongs to the field of chemical products, and relates to a process for separating and purifying 2, 4-diaminotoluene 2, 6-diaminotoluene by TDA, in particular to a process for separating and purifying 2, 4-diaminotoluene by derivatization crystallization method Toluene 2,6-diaminotoluene process. Background technique [0002] Both 2,4-diaminotoluene (2,4-TDA) and 2,6-diaminotoluene (2,6-TDA) are important raw materials for organic synthesis, among which, 2,4-diaminotoluene is not only the It is also an important raw material for the production of toluene diisocyanate (TDI). 2,6-diaminotoluene is an important pharmaceutical intermediate. The method for industrially synthesizing TDA is usually to first nitrate toluene to obtain mixed dinitrotoluene, and then obtain meta-position mixed dinitrotoluene after rectification and separation to remove the ortho-position dinitrotoluene isomers, and then reduce to obtain mixed TDA, wherein Contain...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/51C07C209/86
Inventor 胡雨来王珪武成陈卫权陈贵兴王兴宏赵贤全赵润良
Owner GANSU SHANDAN HONGDINGYUAN CHEM
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