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Preparation and purification method and purification device of dodecyl isocyanate

A technology of dodecyl isocyanate and tolyl isocyanate, which is applied in the preparation of isocyanic acid derivatives, purification/separation of isocyanic acid derivatives, and the preparation of organic compounds, etc.

Pending Publication Date: 2022-04-29
UPCHEM CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, what the existing preparation method obtains is a crude product of alkyl isocyanate, which requires further purification treatment, and there is no purification method for dodecyl isocyanate in the prior art

Method used

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  • Preparation and purification method and purification device of dodecyl isocyanate
  • Preparation and purification method and purification device of dodecyl isocyanate

Examples

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Embodiment 1

[0029] A kind of preparation, purification method of dodecyl isocyanate, described preparation method mainly comprises the following steps:

[0030] 1) Mix dodecylamine and xylene in a mixing tank at a mass ratio of 1:3, and prepare a dodecylamine solution for use;

[0031] 2) Add solid phosgene and xylene at a mass ratio of 1:2 to the reactor, and heat up to dissolve; so that the mass ratio of the dodecyl primary amine to solid phosgene is 1:0.34;

[0032] 3) When the temperature in the reactor reaches 80-100°C, add the dodecylamine solution prepared in the above step 1) dropwise into the reactor, so that the dodecylamine and solid phosgene can form dodecylamine in the xylene medium. Primary amine hydrochloride and unstable intermediate product dodecylmethylamino acid chloride, the intermediate product dodecylamino acid chloride is dehydrochlorinated to obtain dodecyl isocyanate; the time for dropping is 1h, and after the dropping is completed, reflux and keep warm 1.5h; the...

Embodiment 2

[0037] A preparation and purification method of dodecyl isocyanate, the mass ratio of dodecyl amine to xylene is 1:4, the mass ratio of solid phosgene to xylene is 1:3, the mass ratio of dodecyl primary amine to solid The mass ratio of phosgene is 1:0.4. All the other are with embodiment 1. The purification device is the same as in Example 1. The yield of the prepared dodecyl isocyanate is 93%, and the product content is more than or equal to 99.0%.

Embodiment 3

[0039] A preparation and purification method of dodecyl isocyanate, the mass ratio of dodecyl amine to xylene is 1:5, the mass ratio of solid phosgene to xylene is 1:4, the mass ratio of dodecyl primary amine to solid The mass ratio of phosgene is 1:0.5. All the other are with embodiment 1. The purification device is the same as in Example 1. The yield of the prepared dodecyl isocyanate is 95%, and the product content is ≥99.0%.

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Abstract

The invention discloses a preparation method, a purification method and a purification device of dodecyl isocyanate. The preparation method comprises the following steps: 1) preparing a dodecylamine solution in a mixing kettle for later use; 2) adding triphosgene and a solvent into the reaction kettle, and heating for dissolving; 3) when the temperature in the reaction kettle reaches 60-130 DEG C, dropwise adding a dodecylamine solution; the dropwise adding time is 0.5-1.5 hours, and the reflux heat preservation time is 0.5-1.5 hours; the reaction process is monitored by a DCS (Distributed Control System); and carrying out three-stage distillation purification on the obtained dodecyl isocyanate reaction mixed solution. The yield of the obtained dodecyl isocyanate product can reach 95%, and the content of the product is greater than or equal to 99.0%. According to the invention, the low-toxicity chemical triphosgene and the solvent are adopted, and material metering, conveying and operation parameters are all controlled by DCS (Distributed Control System); a one-step method is adopted for synthesis, reaction conditions are mild, and efficiency is high; and a three-stage distillation technology is adopted for purification, so that the product quality and yield are improved.

Description

technical field [0001] The invention relates to a method for preparing and purifying dodecyl isocyanate and a purifying device, belonging to the field of chemical equipment. Background technique [0002] In the prior art, the reaction of organic primary amines and phosgene in an inert solvent is widely used to prepare isocyanates. The phosgene method can be divided into a direct method and a salt-forming method. The direct method is to directly react the primary amine with phosgene to obtain the corresponding isocyanate; the salt-forming method first reacts the corresponding amine with an acid gas such as hydrogen chloride, carbon dioxide, etc. to obtain an amine salt , and then react the amine salt with phosgene. Due to the fast reaction rate of aliphatic amines and phosgene, it is easy to cause amine coating and produce urea by-products in the subsequent thermophotochemical process. As a by-product, the salt-forming photochemical method of making m-xylylenediamine into h...

Claims

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Application Information

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IPC IPC(8): C07C263/10C07C263/20C07C265/04B01D3/00B01D3/10B01D3/14B01D3/32
CPCC07C263/10C07C263/20B01D3/00B01D3/10B01D3/14B01D3/322B01D3/324C07C265/04
Inventor 夏剑锋夏晨东樊晓园陈映波余华胜赖旭明许森挺
Owner UPCHEM CHINA
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