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Method for extracting methyl o-phenylendiamine from TDI organic residue and synthesizing TTA using same

A technology of methyl o-phenylenediamine and toluene diisocyanate is applied in the field of chemistry and achieves the effects of less by-products, low production cost and high purity

Active Publication Date: 2008-07-09
沧州大化新星工贸有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to overcome the deficiencies in the prior art and effectively solve the problem of development and utilization of TDI hydrogenated organic residues, the invention provides a method for extracting toluene diamine from TDI organic residues and using it to synthesize tolyltriazole , so that it has the advantages of simple and convenient process, low production cost, high recovery rate, good product quality, less by-products and high purity, which is conducive to protecting the environment and utilizing resources

Method used

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  • Method for extracting methyl o-phenylendiamine from TDI organic residue and synthesizing TTA using same

Examples

Experimental program
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Embodiment 1

[0024] Take 1700Kg of organic residue with OTD content of 90% in TDI hydrogenation organic residue as an example, and the organic residue is stored in a 200Kg iron drum. The specific extraction process is as follows:

[0025] a. Dissolution process: put 1700Kg TDI organic residue into the chemical material tank 1 first, open the steam heating valve to pass the heat source to the chemical material tank 1, control the water temperature of the chemical material at 85-90°C for 9 hours, after the organic residue is completely dissolved , into the purification distillation still;

[0026] b. Purification and refining process: under the process conditions of controlling the temperature of the organic residue in the purification and rectification kettle 3 to 172°C and a vacuum degree of 200Pa, the ratio of receiving and reflux is controlled to be 6.0:4.5, and the content of the received methyl o-phenylenediamine is more than 99.2%. , a total of 1516Kg of methyl-o-phenylenediamine pro...

Embodiment 2

[0028] Taking 2520Kg of organic residue with an OTD content of 97% in TDI hydrogenation residue as an example, the specific extraction process is as follows:

[0029] a. Dissolving process: put 2520Kg TDI organic residue into chemical material tank 1 first, open the steam heating valve to pass heat source to chemical material tank 1, control the water temperature of chemical material at 90°C for 7.5 hours, after the organic residue is completely dissolved, sent to the purification and rectification process;

[0030] b. Purification and refining process: under the process conditions of the temperature of the organic residue in the purification and rectification kettle 3 of 175° C. and a vacuum degree of 180 Pa, the receiving and reflux ratio is controlled to 7.2: 3.8, and the content of the received methyl o-phenylenediamine is more than 99.4%. A total of 2430Kg of methyl-o-phenylenediamine product with a content of 99.43% was extracted, and the recovery rate was 99.41%. It too...

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Abstract

The invention provides a method of extracting methyl o-phenylenediamine from TDI organic bottom and synthesizing TTA by it, solving development and utilization problem of TDI organic bottom. Using TDI organic bottom as raw material, in a certain temperature and pressure, using the method of dissolution and vacuum extract distillation to extract methyl o-phenylenediamine from TDI organic bottom, medium pressure one-step synthesizing methylbenzene-trinitrogen azoles sodium salt by extracted methyl o-phenylenediamine and excess erinitrit solution, and then by acidification, poaching, vacuum hydroextraction, distillation and purification to produce methylbenzene-trinitrogen azoles TTA product. The material temperature of TDI organic bottom in purification process is 160-190deg C,the evacuation in still is 50-380Pa,the synthesized process of TTA is in temperature 250+-20deg C, pressure 4.6-5.2Mpa, synthesis reacting for 3.5-4h in constant temperature and constant pressure. It is adapted for comprehensive development and utilization of organic bottom, environmental conservation and resoure utilization.

Description

technical field [0001] The invention relates to a process for extracting chemical raw materials from chemical industry residues and its utilization in the field of chemical technology, in particular to extracting methyl-o-phenylenediamine from TDI organic residues and using it to synthesize tolylbenzotriazole TTA method. Background technique [0002] With the development of the chemical industry and the rapid advancement of science and technology, the comprehensive development and utilization of chemical industry residues is becoming more and more important. In the known technology, the industrialized production process of TDI (toluene diisocyanate) is mainly divided into processes such as nitration, hydrogenation and photochemistry of toluene. The products are ortho-, para-isomers and a small amount of meta-isomers. When the ortho- and para-position nitrotoluene undergoes two-stage nitration, the raw materials required for the production of TDI-2,4 or 2,6-dinitrotoluene ar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/18C07C209/86C07C211/51
Inventor 陈淑霞刘华光
Owner 沧州大化新星工贸有限责任公司
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