Method for preparing 2,4-toluene diamino menthyl formate

A technology of methyl toluene dicarbamate and diaminotoluene, applied in the preparation of 2, to achieve the effect of mild reaction conditions and convenient operation

Inactive Publication Date: 2004-04-14
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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And provide catalyst regeneration method

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  • Method for preparing 2,4-toluene diamino menthyl formate
  • Method for preparing 2,4-toluene diamino menthyl formate

Examples

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Effect test

Embodiment 1

[0049] Example 1: 5 g of TDA, 74 ml of DMC, and 0.9 g of zinc acetate were added to the reactor, the reactor was sealed, and the temperature was raised to 120° C. for 2 hours. Continue to raise the temperature to 150°C, and maintain it for 4 hours from the beginning of the temperature rise. Finally, the temperature was lowered to 120°C, and the temperature was maintained for 1 hour from the beginning of the temperature drop, and the reaction was completed. After discharge, filter at 90°C. The filtrate was distilled under reduced pressure, the vacuum degree of the reduced pressure distillation was 7-12mmHg, and the temperature was controlled at 40°C. 9.85 g of product was obtained. The product purity is 95.88%, and the TDC yield is 96.90%.

Embodiment 2

[0050] Example 2: 5 g of TDA, 74 ml of DMC, and 0.6 g of dehydrated zinc acetate were added to the reaction kettle, the reaction kettle was sealed, and the temperature was raised to 110° C. for 3 hours. Continue to raise the temperature to 160°C, and maintain it for 4 hours from the start of the temperature rise, and the reaction ends. After discharge, filter at 70°C. The filtrate was distilled under reduced pressure, the vacuum degree of the reduced pressure distillation was 7-12mmHg, and the temperature was controlled at 50°C. The product 9.72g was obtained. The product purity is 96.8%, and the TDC yield is 96.54%.

Embodiment 3

[0051] Example 3: 5 g of TDA, 55.5 ml of DMC, and 1.0 g of dehydrated zinc acetate were added to the reaction kettle, the reaction kettle was sealed, and the temperature was raised to 120° C. for 2 hours. Continue to raise the temperature to 170°C, and maintain it for 3 hours from the beginning of the temperature rise. Finally, the temperature was lowered to 140°C and maintained for 2 hours from the beginning of cooling. The reaction is over. After discharge, filter at 90°C. The filtrate was distilled under reduced pressure, the vacuum degree of the reduced pressure distillation was 7-12mmHg, and the temperature was controlled at 50°C. The product 9.78g was obtained. The product purity is 98.1%, and the TDC yield is 98.4%.

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Abstract

The invention discloses a producing method of 2, 4-toluene diamino methyl ester formate. It uses zinc acetate as catalyst, it is produced by reacting 2, 4- diamino toluene and dimethyl ester carbonate. The process adopts non-isothermal operation, the reaction is carried on in high pressure kettle uncontinuously. In reaction period, no materials is added in or pulled out, only need to control the temperature, the pressure is correspondent to the temperature. Separates the filtered material, the filtering temperature is control within 60í½90íµ, carries on decompression distillation to the liquid, the vacuum rate is 7í½12mmHg, the temperature is 35í½80íµ, gets the product TDC after instilling out the DMC and carbinol.

Description

technical field [0001] The invention relates to a method for preparing methyl 2,4-toluene dicarbamate. The invention uses zinc acetate as a catalyst to prepare 2,4-diaminotoluene (TDA) and dimethyl carbonate (DMC) by reacting , methyl 4-toluene dicarbamate (TDC), and focus on the recovery and regeneration of process and catalyst, to provide a production method and operating conditions. [0002] 2,4-Toluene diisocyanate (TDI) is an important organic chemical intermediate and an important raw material for the preparation of polyurethane. At present, the production of industrial TDI uses the phosgene method, which is a highly toxic substance, and the by-product of this method is hydrochloric acid, which has a corrosive effect on equipment. Therefore, the research on non-phosgene production of TDI has become the research focus of various countries. At present, the most promising method for industrialization in the production of TDI by the non-phosgene method is: TDA and DMC are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C269/04C07C271/28
Inventor 王延吉王桂荣赵新强李芳
Owner HEBEI UNIV OF TECH
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