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

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 method for extracting chemical raw materials from residues in the chemical industry and its utilization in the field of chemical technology, in particular to extracting methyl o-phenylenediamine from TDI organic residues and synthesizing tolyltriazole by using the same TTA method. Background technique

[0002] With the increasing development of the chemical industry and the rapid advancement of science and technology, the comprehensive development and utilization of residues in the chemical industry is becoming more and more important. In the known technology, the industrial production process of TDI (toluene diisocyanate) is mainly divided into toluene nitration, hydrogenation and photochemical processes. The products are ortho-, para-isomers and a small amount of meta-isomers. When the ortho- and para-nitrotoluenes are subjected to secondary nitration, the raw materials required for the production of TDI are generated-2,...

Examples

Embodiment 1

[0024] Take 1700Kg of organic residue with 90% OTD content in TDI hydrogenated organic residue as an example. 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 in chemical material tank 1 first, open the steam heating valve to pass the heat source into chemical material tank 1, and control the chemical material water temperature at 85~90℃ for 9 hours, after the organic residue is completely dissolved , Sent to the purification and distillation still;

[0026] b. Purification and refining process: under the process conditions of controlling the organic residue material temperature in the purification and rectification kettle 3 at 172°C and the vacuum degree of 200Pa, the ratio of receiving and reflux is controlled to be 6.0:4.5, and the content of received methyl o-phenylenediamine is above 99.2% A total of 1516Kg of methyl o-phenylenediamine product with a content of 99...

Embodiment 2

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

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

[0030] b. Purification and refining process: under the process conditions of the organic residue material temperature in the purification and rectification kettle 3 at 175°C and the vacuum degree of 180Pa, the receiving and reflux ratio is controlled to be 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%....

Technical field

[0001] The invention relates to a process method for extracting chemical raw materials from residues in the chemical industry and its utilization in the field of chemical technology, in particular to extracting methyl o-phenylenediamine from TDI organic residues and synthesizing tolyltriazole by using the same TTA method. Background technique

[0002] With the increasing development of the chemical industry and the rapid advancement of science and technology, the comprehensive development and utilization of residues in the chemical industry is becoming more and more important. In the known technology, the industrial production process of TDI (toluene diisocyanate) is mainly divided into toluene nitration, hydrogenation and photochemical processes. The products are ortho-, para-isomers and a small amount of meta-isomers. When the ortho- and para-nitrotoluenes are subjected to secondary nitration, the raw materials required for the production of TDI are generated-2,...

Examples

Embodiment 1

[0024] Take 1700Kg of organic residue with 90% OTD content in TDI hydrogenated organic residue as an example. 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 in chemical material tank 1 first, open the steam heating valve to pass the heat source into chemical material tank 1, and control the chemical material water temperature at 85~90℃ for 9 hours, after the organic residue is completely dissolved , Sent to the purification and distillation still;

[0026] b. Purification and refining process: under the process conditions of controlling the organic residue material temperature in the purification and rectification kettle 3 at 172°C and the vacuum degree of 200Pa, the ratio of receiving and reflux is controlled to be 6.0:4.5, and the content of received methyl o-phenylenediamine is above 99.2% A total of 1516Kg of methyl o-phenylenediamine product with a content of 99...

Embodiment 2

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

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

[0030] b. Purification and refining process: under the process conditions of the organic residue material temperature in the purification and rectification kettle 3 at 175°C and the vacuum degree of 180Pa, the receiving and reflux ratio is controlled to be 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%....

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