Production process of 1,3-bis(2,4-diaminophenoxy)propane hydrochloride

A kind of diaminophenoxy, production technology technology, applied in the production technology field of 1,3-dipropane hydrochloride, can solve the problem of high impurity content and the like

Inactive Publication Date: 2015-01-21
YIXING XINYU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Purpose of the invention: The purpose of the present invention is to solve the problem that there are many impurities in the finished product of 1,3-bis(2,4-diaminophenoxy)propane hydrochloride produced by the production process of the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A kind of production technology of 1,3-two (2,4-diaminophenoxy) propane hydrochloride, comprises the following steps:

[0018] 1) Add 140 kg of 2,4-dinitrophenol and 31 kg of caustic soda to 500 kg of ethylene glycol diethyl ether solvent, stir and react at 80°C for 1 hour, then control the reaction temperature at 100°C, and drop into the reaction solution Add 75 kg of 1,3-dibromopropane, drop it in about 2 hours, and keep the temperature at this temperature for 5 hours to complete the reaction.

[0019] 2) After the reaction, cool the reaction solution to 5°C, drain the material and filter it with suction, recover the filtrate and use it mechanically, wash the filter cake 5 times with clean water, and the filter cake is the condensation crude product.

[0020] 3) Add 1000 liters of water to the obtained condensed crude product, raise the temperature to 80°C, add liquid caustic soda dropwise to neutralize the pH value to 9, control the temperature at 80°C, and stir for ...

Embodiment 2

[0025] A production process of 1,3-bis(2,4-diaminophenoxy)propane hydrochloride, the following changes are made to step 3) of the production process:

[0026] 3) Add 1500 liters of water to the obtained condensation crude product, raise the temperature to 83°C, add liquid caustic soda dropwise to neutralize the pH value to 9, control the temperature at 86°C, and stir for 2 hours. Rinse again until pH = 7, drain and centrifuge, and dry at 90°C to obtain about 145 kg of condensed product.

[0027] Other steps of embodiment 2 are identical with embodiment 1, finally obtain about 130 kilograms of finished products, content 99.3%.

Embodiment 3

[0029] A production process of 1,3-bis(2,4-diaminophenoxy)propane hydrochloride, the following changes are made to step 3) of the production process:

[0030] 3) Add 200 liters of water to the obtained condensation crude product, raise the temperature to 90°C, add liquid caustic soda dropwise to neutralize the pH value to 10, control the temperature at 90°C, and stir for 2 hours. Rinse again until pH = 7, drain and centrifuge, and dry at 90°C to obtain about 145 kg of condensed product.

[0031] Embodiment 3 Other steps are identical with embodiment 1, obtain about 133 kilograms of finished products at last, content 99.6%.

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Abstract

The invention discloses a production process of 1,3-bis(2,4-diaminophenoxy)propane hydrochloride; based on an original production process, new steps are added in the production process: adding tap water into a reaction pot, starting to stir, then adding a 1,3-bis(2,4-diaminophenoxy)propane hydrochloride condensation product, heating up, then adding liquid caustic soda drop by drop, controlling the temperature and stirring, after stirring is finished, discharging and carrying out suction filtration while being hot, rinsing with clear water, rinsing to a specified pH value, pumping water out and centrifuging, and then drying. The production process can remove impurities fully dissolved in water while the product is not dissolved in water, so the product yield is not decreased, and besides, the impurities required to be controlled are removed.

Description

[0001] technical field [0002] The invention relates to a production process of hydrochloride, in particular to a production process of 1,3-bis(2,4-diaminophenoxy)propane hydrochloride. Background technique [0003] 1,3-bis(2,4-diaminophenoxy)propane hydrochloride is a dye intermediate. In the process of synthesizing 1,3-bis(2,4-diaminophenoxy)propane hydrochloride, impurities that need to be controlled will be synthesized, and the crude product needs to be purified. The purification method of the original 1,3-bis(2,4-diaminophenoxy)propane hydrochloride is as follows: inhale 600 kg of tap water in a 1000-liter reaction pot, start stirring, and then add 1,3-bis( The crude product of 2,4-diaminophenoxy)propane hydrochloride is heated up to 50-60°C to dissolve the material, and then the vacuum is controlled to distill water under reduced pressure at 0.08-0.09mp until the material is precipitated. Stop the distillation, add a certain amount of ethanol when it is cooled to 30...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/84C07C213/02
Inventor 袁顺福宗凯袁郡范琳俞志平
Owner YIXING XINYU CHEM
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