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2, 4-diaminotoluene purification system

A diaminotoluene and crystallizer technology, which is applied in the purification/separation of amino compounds, organic chemistry, etc., can solve the problems of secondary pollution, cannot meet the needs of industrial production, and the yield of molecular sieve method is small, so as to achieve convenient purification and compact structure , the overall effect of small footprint

Active Publication Date: 2015-11-18
CANGZHOU FENGYUAN ENVIRONMENTAL PROTECTION SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the output of the resin method and the molecular sieve method are small, which cannot meet the needs of industrial production, and the residual liquid of the derivatization crystallization method is difficult to handle, which is easy to cause secondary pollution

Method used

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  • 2, 4-diaminotoluene purification system
  • 2, 4-diaminotoluene purification system

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0063] Melt 500kg of 2,4 and 2,6-diaminotoluene mixture (isomerization ratio: 2,4:2,6=80:20) at a temperature of 90°C and pump it into a crystallizer that is also preheated at 90°C Medium; adjust the temperature of the circulating water in the thermostat sleeve, slowly reduce (cooling rate 2°C / h) the temperature of the crystallizer to 65°C, and keep the temperature at this temperature for half an hour, then release the raffinate; adjust the temperature in the thermostat sleeve The circulating water temperature rises slowly (heating rate 4°C / h), and then keeps the temperature for half an hour after reaching 86°C. The sweating liquid collected during the heating process is stored separately from the residual liquid; raise the temperature of the crystallizer to 100°C to melt all the internal materials After that, release the product. 250 kg of a mixture of 2,4-diaminotoluene and 2,6-diaminotoluene (isomerization ratio 95:5) was obtained.

Embodiment 2

[0065] Melt 250kg of the product in Example 1 at a temperature of 100°C, and pump it into a crystallizer at 95°C; adjust the temperature of the circulating water in the thermostat sleeve, and slowly reduce the temperature of the crystallizer (1.5°C / h) to 75°C, And keep the temperature at this temperature for half an hour, then release the residual liquid; adjust the temperature of the circulating water in the thermostat sleeve to increase slowly (2°C / h), and keep the temperature at 98°C for half an hour. Store the residual liquid separately; raise the temperature of the crystallizer to 100°C to melt all the internal materials, and release the product. 200 kg of 2,4-diaminotoluene was obtained, and the purity (GC method) of the product was 99.1%.

Embodiment 3

[0067] Mix 400kg of 2,4 and 2,6-diaminotoluene mixture (isomer ratio: 2,4:2,6=80:20) with 100kg of sweating liquid in Example 1, melt at a temperature of 90°C, Pump into the crystallizer at 90°C; adjust the temperature of the circulating water in the thermostat sleeve, slowly lower the temperature of the crystallizer (1.5°C / h) to 75°C, and keep the temperature at this temperature for half an hour to release the raffinate; Adjust the temperature of the circulating water in the thermostat sleeve to increase slowly (2°C / h), keep the temperature at 98°C for half an hour, store the sweating liquid collected during the temperature rise and the residual liquid separately; raise the temperature of the crystallizer to 100°C, so that After all the internal materials are melted, the product is released. 280 kg of a mixture of 2,4-diaminotoluene and 2,6-diaminotoluene (isomerization ratio 95:5) was obtained.

[0068] In a word, the present invention also has the following advantages at l...

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Abstract

The invention provides a 2, 4-diaminotoluene purification system which comprises a crystallizer, a heat exchanger, a raw material tank, a product receiving tank, a sweat liquid receiving tank and a residual liquid receiving tank. The crystallizer is provided with a feed port and a discharge port. The crystallizer further comprises a temperature adjusting sleeve which is arranged around the crystallizer and used for changing temperature of the crystallizer. The temperature adjusting sleeve is provided with a circulating water inlet and a circulating water outlet. The heat exchanger is used for heating or cooling circulating water in the temperature adjusting sleeve. The raw material tank is communicated with the feed port of the crystallizer. The product receiving tank, the sweat liquid receiving tank and the residual liquid receiving tank are communicated with the discharge port of the crystallizer. The purification system can carry out TDA purification conveniently, the structure is compact, and therefore the overall occupied area is small.

Description

technical field [0001] The invention relates to a technology for purifying 2,4-diaminotoluene from mixed diaminotoluene (TDA). Background technique [0002] 2,4-diaminotoluene is an important dye intermediate and an important raw material for the production of toluene diisocyanate (TDI). The method of 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 ortho-position dinitrotoluene, and then reduce to obtain mixed TDA, 2,4- The content of TDA and 2,6-TDA mainly has two ratios (mass isomerization ratio): about 80:20 or about 65:35. Because the quality of dyes synthesized by pure 2,4-TDA is better, and the performance of polyurethane polymerized with pure 2,4-TDA is better, so the economical and efficient purification of 2,4-TDA has a broad industry prospect. [0003] At present, although there are related reports on the preparation o...

Claims

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Application Information

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IPC IPC(8): C07C211/51C07C209/84
Inventor 苏德水朱建华黄津于建才王长飞
Owner CANGZHOU FENGYUAN ENVIRONMENTAL PROTECTION SCI & TECH
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